Professional Documents
Culture Documents
Sampling Handbook
Revision 1.0
April 2013
Preface
This handbook provides basic guidance for working-level environmental field sampling personnel to
ensure the integrity of monitoring activities tied to regulatory reporting requirements. The handbook
was developed as a tool for Department of Defense (DoD) personnel. In cases where a contractor
provides environmental sampling and field testing services, the contractor is responsible for ensuring
self-compliance with all environmental and occupational safety and health laws and regulations. In
certain instances, special requirements may dictate a more rigorous detail, depending on federal, state,
and local regulations. Local field sampling procedures should be compatible with the contents of this
handbook. However, there is no intent for guidance herein to replace standard operating procedures,
which may exist at the local level.
Issues regarding the contents of this handbook should be brought to the attention of the DoD Environmental Data Quality Workgroup, Field Sampling and Testing Subgroup.
The DoD Environmental Data Quality Workgroup (EDQW) developed this handbook to provide guidance for environmental field sampling personnel and laboratories performing services for the DoD. It is
based on the Navy Environmental Compliance Sampling and Field Testing Procedures Manual (August
2009), and is expanded to incorporate DoD-wide field sampling and testing guidance. Nothing in this
document relieves any field or laboratory personnel from complying with more stringent contract specifications, host-nation final governing standards, or federal, state, and local regulations. This handbook
can and should be supplemented by project-specific requirements. The DoD EDQW strongly encourages project teams to involve laboratories, project chemists, and field personnel during projectplanning activities. The involvement of the laboratories, field personnel, and project chemists is critical
to the development of project-specific measurement performance criteria (MPC) and to the selection of
methods capable of satisfying the MPC.
Preface
Table of Contents
ii
TABLE OF CONTENTS
Preface ....................................................................................................................................................................... i
Chapter 1. Introduction ......................................................................................................................................... 1-1
1.1. Purpose ................................................................................................................................................. 1-1
1.2. Scope .................................................................................................................................................... 1-1
1.3. Background .......................................................................................................................................... 1-1
1.4. Requirements for Laboratory Testing.................................................................................................. 1-1
1.4.1. Compliance Testing ......................................................................................................................... 1-2
1.4.2. Restoration Testing .......................................................................................................................... 1-2
1.5. Handbook Overview ............................................................................................................................ 1-2
Chapter 2. Sampling and Field Testing Program Overview................................................................................ 2-1
2.1. Purpose ................................................................................................................................................. 2-1
2.2. Need for Proper Planning..................................................................................................................... 2-1
2.3. Systematic Planning and the Conceptual Site Model (CSM) ............................................................. 2-1
2.4. Aerial Photo and Map Analysis ........................................................................................................... 2-2
2.5. Fate and Transport................................................................................................................................ 2-3
2.6. Geophysical Exploration ...................................................................................................................... 2-3
2.7. Data Quality Objectives (DQO) Process ............................................................................................. 2-3
2.7.1. Sampling Strategy ............................................................................................................................ 2-4
2.7.2. Selecting a Sampling Design ........................................................................................................... 2-5
2.7.3. Background Samples ....................................................................................................................... 2-7
2.7.4. Collecting Effective Data ................................................................................................................ 2-9
2.8. Selecting the Project Team .................................................................................................................. 2-9
2.9. Developing a SAP .............................................................................................................................. 2-10
2.10. Health and Safety Plan....................................................................................................................... 2-11
2.10.1. Service-Specific Safety and Occupational (SOH) Health Program ........................................... 2-11
Chapter 3. Common Sampling Procedures .......................................................................................................... 3-1
3.1. Purpose ................................................................................................................................................. 3-1
3.2. Preparations for Field Sampling .......................................................................................................... 3-1
3.2.1. Preparing for a Sampling Event ...................................................................................................... 3-2
3.2.2. Preliminary On-Site Evaluation ...................................................................................................... 3-3
3.2.3. Preliminary Site Safety Evaluation ................................................................................................. 3-3
3.2.4. Explosive Safety Evaluation............................................................................................................ 3-4
3.2.5. Preliminary Sampling Evaluation ................................................................................................... 3-4
3.3. The Sampling Event ............................................................................................................................. 3-4
3.4. Sampling Procedures............................................................................................................................ 3-4
3.4.1. Sampling Strategies ......................................................................................................................... 3-5
3.4.2. Sampling Procedure Checklist ........................................................................................................ 3-5
3.5. Sample Documentation and COC Procedures..................................................................................... 3-6
3.5.1. Pre-Assigned Sample Numbers ....................................................................................................... 3-6
3.5.2. Sample Container Labeling ............................................................................................................. 3-7
3.5.3. FLB/FN ............................................................................................................................................ 3-7
3.5.4. Field Notes/Field Sampling Forms ................................................................................................. 3-9
3.5.5. Chain of Custody (COC) ............................................................................................................... 3-10
3.5.6. Request for Analysis ...................................................................................................................... 3-16
3.6. Sample Packaging, Handling, and Transportation ............................................................................ 3-16
3.6.1. Sample Packaging Requirements .................................................................................................. 3-17
3.6.2. Marking and Labeling.................................................................................................................... 3-23
Table of Contents
iii
Table of Contents
iv
Table of Contents
vi
vii
viii
ix
Table of Contents
Chapter 1. Introduction
1.1. Purpose
The purpose of the DoD Environmental Sampling
Handbook is to provide general sampling guidance and promote consistency in how environmental samples are collected and analyzed. The
handbook discusses strategies and techniques that
can be employed to sample and analyze various
media, including but not limited to water, soils,
gas, and tissues. Applications and limitations of
each sampling strategy and technique are briefly
described. This handbook is not intended to be
all inclusive, but it does provide guidance and
discussion of basic sampling techniques. Many
of the techniques discussed in this handbook have
been derived from approved and accepted regulatory programs. When appropriate, references to
standardized methods are provided.
1.2. Scope
This handbook describes techniques that can be
used for environmental sampling and analysis at
Department of Defense (DoD) compliance, restoration, or other sites. Handbook users are cautioned on possible differences between material
presented here and requirements contained in
control documents such as permits, licenses, state,
local, and other countries program regulations.
These control documents have legal precedence
and may prescribe sampling practices unique to a
specific program or site. When sampling to
document compliance with a control document
(regulation, permit, etc.), the control document
takes precedence over this handbook, and this
handbook should be used as a guidance document
only.
1.3. Background
Accurate, defensible, environmental sampling
and field-testing results are imperative for regulatory compliance monitoring. There is great opportunity for error considering the variable conditions within the environment and the great variety
of sampling equipment available. There is little
tolerance for error since the validity of associated
laboratory test results depends on
Chapter 1 Introduction
CWA
TSCA
SDWA
FIFRA
CAA
Note: The Emergency Planning and Community Right-toKnow Act (EPCRA) and Executive Order 12856 may place
some additional demands on the laboratories.
These laws prescribe analyses of potable and non-potable
water systems, hazardous and toxic materials, and air
emissions. To comply with these regulations, the DoD
operates its facilities pursuant to regulatory requirements
that address process discharges. Permits may be required
for base support systems (dry docks, sewer, water, industrial waste treatment) and production processes (painting,
degreasing, abrasive blasting, flushing). The DoD accomplishes environmental analysis through both in-house and
commercial laboratories.
Chapter 1 Introduction
CERCLA
Comprehensive Environmental
Response, Compensation, and Liability Act
SARA
RCRA
Page 1-2
Chapter 1 Introduction
Page 1-3
Chapter 8
Groundwater Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times
Chapter 6
Surface Water
Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times
Chapter 5
Aquatic Sediment
Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times
Chapter 10
Waste
Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times
Chapter 3
Common Sampling
Procedures
Chapter 1 Introduction
Chapter 11
Air Sampling
Chapter 12
Process Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times
Chapter 4
Soil Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times
Appendix A
Sampler/Sampling
Recommendations and
Strategies
Chapter 9
Drinking Water
Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times
Chapter 14
Guidelines
for
Requesting
Laboratory Testing
Appendix B
Requirements for Sample
Containers, Preservation,
and Holding Times
Appendix C
Requirements for Collections
of Quality Control Samples
Page 1-4
Chapter 1 Introduction
Page 1-5
Although the benefits of using a dynamic sampling strategy are substantial, they are not applicable for all situations. Dynamic sampling activities often need more extensive planning up front
than traditional staged or static field activities.
Successful dynamic sampling plans should prepare not only for what is known about a site, but
also for possible conditions that could affect the
completion of the fieldwork. Quick turnaround
analysis is typically needed to facilitate dynamic
field activities. If on-site or rapid off-site analysis
is not economically or technically feasible, a
static sampling strategy may be more appropriate.
Dynamic field activities also need more field
oversight, because the regulator should be involved in evaluating key technical decisions as
they occur. In addition, dynamic sampling routinely requires the presence of one or more experienced technical staff in the field. Experienced
staff plays a key role in the decision-making
process, and their recommendations can greatly
influence the direction field activities take. If an
experienced technical team leader is not available
to oversee the fieldwork, dynamic sampling will
often be an ineffective method for data collection.
In this case, a static sampling strategy, which
allows time for review and careful consideration
by technical experts not available for on-site
activities, may be more appropriate.
For additional information on the dynamic sampling process refer to EPA/540/R-03/002
(http://www.epa.gov/superfund/programs/dfa/do
wnload/guidance/40r03002.pdf).
2.7.2. Selecting a Sampling Design
One of the primary objectives of systematic
planning and the DQO process is to determine the
data quality and quantity needed to address
project objectives. Once the data requirements
are identified, the next step in the process is to
develop a sampling design or methodology that
specifies the number, type, and location (spatial
or temporal) of the samples to be selected for
measurement.
There are two main categories of sampling designs: statistical and non-statistical. Statistical
Page 2-5
worst case or those of the highest concentrations. Sampling locations are selected based on
visual signs of contamination or previous knowledge about the site. Using a biased sampling
design is most appropriate when dealing with a
known contamination source. The disadvantage
of biased sampling is that contaminated areas
may be overlooked due to inadequate knowledge
of the site or a lack of visual signs of contamination.
For additional information on sampling designs
for environmental data collection, see
EPA/240/R-02/005 QA/G-5S:
http://www.epa.gov/quality1/qs-docs/g5sfinal.pdf).
Visual Sample Plan (VSP) is a software tool that
can be used to employ several of the sampling
strategies previously discussed. VSP supports the
implementation of the DQO process by displaying different sampling plans, linking them to the
DQO process, and then determining the optimal
sampling specifications to protect against potential decision errors.
This easy-to-use program is highly visual, very
graphic, and intended for use by non-statisticians.
The VSP software program may be downloaded
from http://vsp.pnnl.gov/.
2.7.3. Background Samples
In accordance with U.S. EPA guidance, background (reference area) sampling is conducted to
distinguish site-related contamination from naturally occurring or other non-site-related anthropogenic chemicals (EPA, 1989). Background
chemicals can be either localized or widespread
and should be evaluated during site investigations
in order to differentiate between Defense Environmental Restoration Program cleanup responsibilities for site-related releases and background
conditions and/or non-site-related anthropogenic
sources. Both naturally occurring and non-siterelated anthropogenic background levels of chemicals should be established and considered as
early as the Preliminary Assessment/Site Inspection (PA/SI) phase of the CERCLA process or the
Resource Conservation and Recovery Act
Page 2-7
Effective data reinforce a more productive conceptual framework for data generation by encouraging critical thinking about the anticipated role
of data. Focusing on achieving effective data
forces the systematic planning process to answer
the following questions:
Page 2-11
Page 2-12
Page 3-1
WARNING: When using containers filled with preservative, use caution when filling the bottles to ensure the
preservative is not released to the environment and the
correct amount of preservative has been added to adequately fix the sample.
Page 3-2
Note: When in use, sampling equipment should be anchored to prevent loss in the event the rope or equipment
slips through the hands of the sample collector.
Page 3-3
3.3.
Page 3-4
Sampling Approach
- Objective
- Design of sampling plan
- Statistics
Material to be Sampled
- Physical state
- Volume
- Hazardous properties
- Composition
Site
- Accessibility
- Waste generation and handling
- Transitory events, startup, shutdown
- Maintenance
- Climate
- Hazards
Equipment
- Maintenance
- Preparation and cleaning
- Operation
- Calibration and standardization
Sample Handling, Transportation, Storage
and Preservation
- COC
- Seals
- Forms
- Containers
- Preservatives, reagents, and supplies
QA/QC
- Controls on process
- Audits
- Training
- Samples, blanks, duplicates, and
spikes
Health and Safety
- Personnel protection
Page 3-5
- Safety procedures
- Emergency procedures
Laboratory
- Document transfer
- Sample arrival schedule, transfer
- Sample preservation, handling and
storage
- Analytical methods and QC
- Reporting format and schedule.
3.5. Sample Documentation and COC
Procedures
Thorough documentation of a samples custody is
required to support sample validity. The documentation must verify that the samples are representative, were collected in accordance with the
requirements of the SAP, and are not vulnerable
to tampering before being received by the laboratory. The COC begins when the sample is taken and
ends when the sample is disposed of. Sample
documentation and COC procedures include the
following.
A completed sample collection label attached to
all sample containers
Records of sampling operations written in
FLB/FN or related forms as designated for the
operation in the SAP. Records include sample
type, sample matrix, sampling method, field test
methods, and QC procedures. A table may be
used to present this information.
Identification of every sample container on a
COC record and all custody transfers
documented
Custody of the samples with all discrepancies in
the field operations resolved or duly recorded.
The following should be used to generate the required sample documentation.
________________________________________
Note: EPAs Field Operations and Records Management
System II Lite (FORMS II LiteTM) software is an electronic COC and may also be used to simplify and accelerate the
sample documentation process.
Page 3-6
PROJECT NAME
Sample #: XXXXX
Container #: XXXXX
Sample #:
_______________
Date: ______
Time: _________
Location:
________________
Cont. Size:
________________
Cont. Type:
________________
Matrix:
________________
Type of Sample: _______________
Preservative:
________________
Signature:
________________
3.5.3. FLB/FN
The FLB/FN is the written record of all field data,
observations, field equipment calibrations, and
sample collection activities. Potential for future
legal actions dictates that the FLB/FN be sitespecific and that they be hardbound (e.g., ledger,
composition book, diary, etc.). All pages (front
and back) shall be serially numbered so removal
will be apparent. Samplers shall adhere to the
following guidelines when using FLB/FN.
Page 3-8
Page 3-10
PROJECT:
EPA ID NO:
Proj./Task No.
Date:
Weather:
Samplers:
WELL ID:
Well Condition:
Well Riser Dia. (ID):
Screened Interval:
S.W.L. Measuring Pnt:
Well Bottom Depth:
QC
MS/MSD
Blank
Instrumentation/Equipment Data:
Sample ID
Analysis
Primary
QC
MS/MSD
Calibration Date:
Units
C
ms/cm
ppm
____
Minutes
____
Minutes
____
Minutes
____
Minutes
mg/L
mg/L
mg/L
mg/L
Floating Product:
Sheen:
Minutes
Minutes
Minutes
Minutes
____
Minutes
____
Minutes
____
Minutes
____
Minutes
mV
NTU
Page 3-11
Page 3-12
Page 3-13
Page 3-14
the laboratory or agency shall request the representatives signature acknowledging sample
receipt. If the representative is unavailable or
refuses to sign, this is noted in the received by
space.
Field COC terminates upon laboratory receipt of
the samples. The laboratory should complete the
received by sections and if appropriate, the
preservative checks sections on the COC record
and return the original signed record to the Program Manager. If there are any discrepancies
between the COC record, the contents of the
shipping container, and the SAP or contract
requirements provided to the laboratory, the
samples in question shall be segregated from
normal sample storage, and the laboratory shall
immediately notify the Program Manager. In
some cases, the laboratory checks the sample
submittal and recordkeeping to ensure adherence
to the SAP. This added check is often used in
drinking water and wastewater testing programs
for compliance monitoring. Recordkeeping and
information checks should be performed by the
laboratory to ensure the samples received meet
the requirements of the SAP.
3.5.5.3. Custody Seals (Optional)
Custody seals are narrow strips of adhesive paper
used to indicate whether a shipping container has
been opened during shipment. The seals are
placed along the edges of the most exterior container in which samples are enclosed. It is not
always necessary to place seals on individual
sample containers in the shipping container.
Paper custody seals should be signed and applied
before the shipping container is shipped to the
laboratory. The preferred procedure includes use
of a custody seal attached to the front-right and
back-left of the container. Custody seals are
covered with clear plastic tape. Another way to
use custody seals, is to put all sample containers
with packing and ice in a large garbage bag and
seal the garbage bag with a signed custody seal.
3.5.5.4. Custody Transfer
Transfer of custody and shipment procedures are
as follows.
Page 3-15
should be made based on knowledge of the material. Samples requiring special packaging or
labeling are those containing chemicals that are
listed as hazardous materials in:
49 CFR 172.101
CERCLA RQ Hazardous Substances
DOT CLASS 9 listed in 49 CFR 172.101
Appendix A, Poison DOT Class 6.1 and
Flammable Liquids.
Environmental (non-hazardous) samples are those
that are not classified as Hazardous Materials
under DOT regulations, are packaged in quantities less than the CERCLA RQ, and for which a
Hazardous Waste Manifest is not required by
EPA. These samples require careful packing, but
no special shipping procedures. In general, samples of groundwater, surface water (other than
leachate or lagoons), and soil may be shipped as
environmental samples (non-hazardous) to an
analytical laboratory for testing if each of the
sample containers contains less than 1 pound of
soil or 1 gallon of water, and the entire shipping
package weighs less than 66 pounds. Eventual
analysis for a hazardous constituent does not
necessarily classify a sample as a DOT hazardous
material, nor does the classification of a material
as a hazardous waste under EPA regulations.
DOT regulations forbid the shipping of nonhazardous materials as hazardous. However, if
any doubt exists as to whether the sample might
be classified as a hazardous material, the sample
should be treated as hazardous.
Note: For details on the shipping of non-hazardous waste,
refer to ASTM D6911-03: Standard Guide for Packaging
and Shipping Environmental Samples for Laboratory
Analysis. This standard provides guidance in determining
the most appropriate procedures for packaging and shipping
environmental samples.
Page 3-17
trichloroethylene, trichlorobenzene, PCB transformer oil, and many of the other poisonous
materials commonly encountered.
3.6.1.3. CERCLA Reportable Quantities
DOT Class 9
Table 3-2 Column 3 lists packaging procedures
for substances (liquids and solids) where the
waste material is not otherwise classified as a
DOT Hazardous Material because of hazardous
properties and for which the entry in Column 8a
of 49 CFR 172.101 Table is 155. For the shipment of larger quantities of EPA hazardous waste
and DOT Class 9 hazardous substances where the
quantity of material in each container exceeds the
CERCLA RQ and no other DOT Hazardous
Material classification applies, the following
packaging requirements apply:
Page 3-18
Nonhazardous
Samples
Hazardous
Samples
1*
1*
Write the sample number on the can lid. Indicate This Side Up
by drawing an arrow on the can.
Place cans in the container and fill the remaining volume of the
shipping container with packing material. Add ice bags if
required.
Place the sample containers top-up in the shipping container.
Arrange the sample containers so that glass containers are
surrounded by plastic containers.
Fill the void space around and on top of the sample containers
with plastic bags filled with ice cubes or ice chips.
Seal the COC record in a clear plastic resealable food bag and
tape it securely to the inside of the shipping container lid.
10
11
Page 3-19
By Common Carrier
Instructions
Nonhazardous
Samples
Hazardous
Samples
12
13
14
15
Place a This End Up label on the lid and on all four sides of the
shipping container.
10
11
Affix the signed and dated custody seals on the front right and
back left of the shipping container. Cover the seals with wide,
clear tape.
*Numbers indicate the instructions that must be followed.
16
17
Page 3-20
Flammable
Liquid
66 pounds
DOT Class 9
Poison DOT
Class 6.1
66 pounds
66 pounds
Liquids
4 liters (1 gallon)
Solids
5 kilograms (11
pounds)
Liquids
4 liters (1 gallon)
Solids
5 kilograms (11
pounds)
49 CFR
172.101 Table,
Column 6b
49 CFR
172.101 Table,
Column 5 or
The flash point
of the liquid
1*
1*
1*
Liquids: 3
Solids: 4
Page 3-21
Instructions
Flammable
Liquid
Poison DOT
Class 6.1
DOT Class 9
10
9
Seal the cooler lid with clear tape or
strapping tape. Affix security seals.
*Numbers indicate the instructions that must be followed.
Page 3-22
Sample # or ID
Date of collection
Collector
Analysis requested
Preservative
Sample location.
Sample labels must clearly link the sample to the
field sheet or the COC record and must be written
legibly and in permanent ink. In addition, all
containers must be labeled and listed on the COC
record.
Note: If a three-bottle set is used for VOAs, all three bottles
must be labeled and listed on the COC record.
OSHAs Hazard Communication Standard requires all containers of hazardous materials coming in or out of a workplace to be labeled with the
contents, appropriate hazard warnings, and the
name and address of the manufacturer. OSHA
does not specify a standard labeling method, but
some commonly used ones are provided by National Fire Protection Association (NFPA), Hazardous Materials Identification System (HMIS),
ANSI, and DOT.
3.6.3. Shipping Papers
Ship high hazard samples via overnight courier
following the couriers documentation requirements. A special airbill must be completed for
each shipment. An EPA manifest must be prepared if the shipping container contains hazardous waste unless the samples are exempt. The
Hazardous Waste Manifest must bear the
handwritten signatures of the generator, transporter, and designated facility. A copy of the manifest must be kept for 3 years by the shipper. The
shipping papers must contain the name, address,
and handwritten signature of the shipper.
The shipping papers (and Hazardous Waste Manifest if used) must contain a 24-hour emergency
response telephone number. This phone number
must be monitored at all times while the hazardous material is in transportation, including storage
incidental to transportation. The phone must be
monitored by a person who is either knowledgeable of the hazards and characteristics of the hazardous material being shipped and has comprehensive emergency response and incident mitigation information for that material, or who has
immediate access to a person who possesses such
knowledge and information. The emergency
response phone number must be entered on the
shipping paper immediately following the description of the hazardous material or entered
once on a shipping paper if the number applies to
all of the hazardous materials and is indicated for
emergency response information.
3.7. QA/QC Protocol
QC is a normal part of good field and laboratory
practice. QC includes all of the procedures apPage 3-23
3.7.1.
Decontamination of Sampling
Equipment
The SAP should address the extent of decontamination and specify the procedures to prevent
sample contamination. Sampling may be performed using separate laboratory cleaned equipment for each sample location. Procedure effectiveness should be checked for each matrix by
submitting equipment decontamination blank
samples to the laboratory for analysis.
Note: For specific information regarding the decontamination of field equipment, refer to ASTM D5088-02, Standard
Practices for Decontamination of Field Equipment Used at
Waste Sites. This standard describes the decontamination
process for field equipment used in the sampling of soils,
soil gas, sludges, surface water, and groundwater at waste
sites. According to this standard, these practices are applicable only at sites where chemical (organic and inorganic)
wastes are a concern, not for radiological, mixed (chemical
and radiological), or biohazard sites.
3.7.2.
3.7.3.
3.7.4.
3.7.7. QC Samples
Field QC samples are prepared and analyzed to
determine whether test samples have become
accidentally contaminated, check on the repeatability of the method, and ensure the samples are
representative of the site or matrix sampled. A
number of different QC samples may be specified. Each of the QC samples checks for a potential problem that can affect data reliability. The
recommended frequency for each type of QC
sample is summarized in Appendix C.
Page 3-25
sampling site and returned to the laboratory without being opened. This serves as a check on
sample contamination during sample transport
and shipping.
Note: The caps used on VOA vials have Teflon-lined
septa. The Teflon side of the silicone septum should face
the sample. Prior to closing a vial, make sure there is no
soil particle or dirt on the sealing surface of the VOA vial to
prevent leaks. If a high concentration of volatile chemicals
is present in the air in a shipping container, these chemicals
can pass through the septum and contaminate the sample.
A trip blank is included in each shipping container used to ship VOA water samples. One VOA
trip blank (two vials) is submitted to the laboratory in each cooler or per sampling event. The
frequency of collection for trip blanks is specified
in the SAP and is based on the data quality needs.
Trip blanks are assigned container numbers from
the same sequence used for the test samples, and
are not designated as blanks on the COC record.
3.7.7.6. Matrix Spike (MS)/Matrix Spike
Duplicate (MSD)
Project or compliance QC procedures require that
the laboratory spike a portion of the matrix with a
predetermined quantity of analyte(s) prior to
sample extraction/digestion and analysis. The
frequency of performing an MS is dependent on
the data quality needs and method requirements.
A spiked sample is processed and analyzed in the
same manner as the sample. The result of the
analysis of the spike compared with the non-spike
sample indicates the ability of the test procedures
to recover the analyte from the matrix, and provides a measure of the performance of the analytical method executed by the laboratory.
For an MSD, a second portion of the matrix is
spiked, and the recovery of the MSD can be
compared with the recovery of the MS.
Depending on the matrix and analysis, additional
sample containers may be specified to provide
enough material for this laboratory procedure.
These sample containers are assigned container
numbers from the same sequence as the test
samples and are designated MS/MSD materials
on the COC record.
Field Records
- COC records
- Sample container labels
- FLBs or field forms
- Personnel training records
Sampling Procedures
- Equipment
- Sample containers
- Accuracy of sample location
descriptions
- Comparability of field sampling
techniques
- Collection and preparation of QC
samples
- Sample preservation
- Equipment decontamination
- Contaminated waste storage and
disposal
Page 3-27
Markers
Coolers
Ice
Packing material
Packaging tape
COC form
Custody seals (if required)
Decontamination storage containers,
equipment, and materials
Personal safety equipment, safety test
equipment
Field screening or testing equipment,
standards, reagents, and SOP
Testing field forms or logbooks
Laboratory instructions (if different from
custody form).
Page 3-28
Page 4-2
The rate at which groundwater will cause contaminants to spread is affected by both the speed at
which the groundwater moves through the soil
Chapter 4 Soil Sampling
and the extent to which the soil absorbs the contaminants. One of the most serious effects of
accidental spills and improper disposal of hazardous chemicals is contamination that precludes the
use of a groundwater source for drinking water.
4.3.2. Site-Specific SAP
A soil sampling program should collect soil
samples at a specific locations and depths that are
representative of the site. Procedures that result
in the collection of an undisturbed soil column
will yield the most representative soil samples.
The development of a site-specific SAP is the
first step toward collecting a representative soil
sample (see Chapter 2 for a detailed discussion of
SAP development applicable to all sampling
programs). Each SAP is an instruction manual
for field personnel, and should be built around the
objectives and sampling strategy. The discussion
below focuses specifically on SAP development
for soil sampling programs.
Ideally, the SAP should be based on knowledge
of which contaminants are likely to be present
and how the distribution of the contaminants may
be affected by the soil characteristics of the site.
The purpose of the fieldwork also may be to
define the soil characteristics and obtain chemical
data for determining compliance with federal,
state, or local requirements. It is possible for soil
sampling to be conducted in a number of phases,
with the field observations and field test results
providing data to guide subsequent work. If
knowledge of contaminants and site soil characteristics is limited, then dynamic sampling techniques and field measurements can be used to
locate sampling points.
Dynamic sampling relies on individuals in the
field to interpret field data as it becomes available
and revise the sampling strategy accordingly.
Dynamic sampling can quickly provide significant amounts of information needed to develop
the conceptual model for the site. Dynamic
sampling in many instances, however, is considered a first step toward developing a more focused soil sampling program for a particular area
within the site.
Page 4-3
Page 4-5
considerations are required when sampling explosive wastes that are susceptible to shock, friction,
electromagnetic radiation, electrostatic discharge,
sparks, flames, elevated or freezing temperatures,
moisture, or sunlight. Failure to handle explosives correctly could result in damage to property,
injury, or loss of life. For explosives safety and
handling requirements, refer to DoD 6055.09-M,
DoD Ammunition and Explosives Safety Standards. For Navy projects, also refer to NAVSEA
OP5, Volume 1, Ammunition and Explosives,
Ashore Safety Regulations for Handling, Storing,
Production, Renovation, and Shipping.
The collection of quality soil sampling data requires documentation of site surface conditions
(e.g., locations of buildings, pavement, standing
water, seeps, sediment runoff, discolored soil)
and subsurface conditions such as depth of various layers of soil, depth to groundwater and
bedrock at different locations. The chemical data
obtained from the analysis of soil samples is
useful only within the context of these site conditions, so it is imperative that the exact location of
each sample be documented and the soil samples
accurately represent the conditions at the site.
traditional computer aided design (CAD) procedures. GIS-based data analysis is quicker, easier,
and more accurate compared with traditional
CAD methods. GIS can be used to analyze site
conditions such as depth to groundwater, saturated thickness, hydraulic conductivity, and soil
type for selection of suitable sampling points as
well as for analyzing relationships between sample locations, tracking sampling points, and relocating sampling points under changing site conditions.
The basic tools necessary for incorporating a GIS
into a sampling program include a global positioning system (GPS) unit/receiver and a computer program such as the ESRIs ArcGIS. The GPS
receiver is used to locate predetermined sampling
points in the field and/or record the location of
sampling points as samples are collected. The
GIS program can be used to analyze site conditions prior to the sampling event or map and
analyze the collected data. Creating a GIS database at the early stages of the sampling process
provides for an effective method for data management, analysis, and presentation. The use of a
GIS can significantly streamline many aspects of
a soil sampling program and facilitate the exchange of resultant data among stakeholders.
Site maps, whether prepared using GIS- or CADbased systems, should include surface contour,
surface information, and sampling locations, as
discussed below.
4.5.1.1. Surface Contour
Unless the site is completely flat, it is important
that the surface contour be indicated on the site
map. The depth of soil samples is measured from
the surface, but the surface reference can be lost
due to excavation or filling activities at the site.
If a contour map of the site is not available, it
may be necessary to have one prepared by a
survey team prior to sampling.
4.5.1.2. Surface Information
Sampling personnel should validate the site map
before beginning any sampling activities, noting
Page 4-9
any discrepancies. The following surface information should be recorded if not already shown:
Buildings or structures
Paved areas
Unpaved roads and parking areas
Surface areas with different types of soils,
including fill areas (e.g., gravel roads, clay,
sand, peat)
Standing water, both permanent (e.g., ponds
and streams) and temporary (e.g., persistent
puddles)
Water seeps
Water runoff patterns and accumulations of
runoff sediments
Exposed bedrock
Discolored soil
Stored materials, debris, and soil piles
Vegetation, including distressed vegetation.
Photographs should be taken to document site
surface features. Photography requirements
should be established by the Program Manager to
ensure compliance with the policy and regulations of the facility.
4.5.1.3. Documentation of Sampling
Locations
The location of each sample and the designated
sample numbers should be shown on the site
map. Samples should be collected at the designated sampling points. Depth of samples from
the surface should be recorded. If it becomes
necessary to sample more than 1 foot from the
required location due to interferences from trees,
pavement, subsurface rocks, or buried utilities,
the new sample location should be noted on the
map, and the reason for moving the sampling
location should be explained in the FLB/FN.
4.5.2. Preliminary Tests and Observations
A number of field tests and observations may be
required to document sampling and subsurface
conditions. Such tests may include weather
conditions at the time of sampling, a description
of the subsurface geology, and the presence of
Chapter 4 Soil Sampling
event. Barometric pressure changes can introduce atmospheric air into the shallow vadose
zone, so soil gas should not be sampled during
the passing of a weather front. All of the factors
listed above can affect the ability of contaminants
to be properly sampled. In most cases, adjustments to the sampling strategy can be made to
increase sampling effectiveness.
When soil gas sampling is used to optimize monitoring wells or soil boring locations or monitor
the integrity of USTs, a sampling strategy based
on a judgmental or biased approach is recommended. However, when soil gas sampling is
used for general site reconnaissance, the use of a
statistical sampling method (i.e., a systematic grid
approach) is typically used. Many projects use a
combination of these sampling strategies. For
instance, an initial sampling may be done by a
predetermined regularly spaced grid pattern to
identify the presence of contamination, followed
by a judgmental or close, irregularly spaced grid
pattern approach to refine the delineation of the
contamination detected. Grid spacing shape and
size should be based on the project objectives and
allowable uncertainty in the decision-making
process, but be flexible enough to allow modifications in the field to account for site characteristics, or generated results.
Soil gas samples may be generated in conjunction
with an active or passive sampling system. An
active soil gas sampling system involves the
forced movement of bulk soil gas from the vadose zone to a collection device through a probe
or similar apparatus by the influence of a vacuum
source. The air within the system may be monitored real-time through a sample port with an
appropriate detector (e.g., photoionization detector (PID) or flame ionization detector (FID)).
Active soil gas systems may also be sampled with
a gas-tight syringe, Tedlar bags, glass bulbs,
Summa canisters, or other containment devices
for subsequent onsite or off-site analyses.
The active soil gas sampling system may also be
configured to collect a sorbent sample. In this
type of system, the probe is connected to a collecChapter 4 Soil Sampling
Page 4-12
It is important that soil samples consist of reasonably undisturbed soil from the specified sampling
depths. Access to the soil often requires drilling
or excavation down to the specified depth. In
some cases, it may be necessary to use a jackhammer to remove either concrete or pavement
from the sampling locations. In instances where
areas are grass-covered and no surface sample is
required, several square feet of sod should be
carefully cut away. A decontaminated stainless
steel shovel should be used to carefully remove
the turf so that it may be replaced when sampling
is complete. The stainless steel shovel should be
decontaminated between sampling locations.
Turf also can be removed by hand from sample
locations, provided that personnel wear clean
nitrile or PVC gloves.
4.6.1. Surface Samples
Soil samples should be taken from undisturbed
soil, not from material that is temporarily lying on
the ground. Unless the SAP specifically requires
the sampling of surface debris, remove organic
debris such as leaves, and accumulated trash or
demolition rubble, to expose the soil. The SAP
should define the depth of surface samples. Specific state and local compliance programs may
define surface samples as the first 3, 6, or 12
inches below the vegetation layer. Note in the
FLB/FN how much and what kind of material is
removed. Surface samples can be collected using
stainless steel trowels, spoons, or bucket augers.
Chapter 4 Soil Sampling
A variety of tools, ranging from handheld methods to larger fuel-powered methods, can be
used to access unconsolidated soils. Consolidated
soils can be difficult to sample because they are
difficult to penetrate. Different drilling methods
can be used to access consolidated soils. Truckmounted drill rigs can gain access to soil at any
reasonable depth and can penetrate hard layers.
When used with a hollow-stem auger, a drill rig
can retrieve reasonably undisturbed cores for
classification purposes. The following subsections describe the various techniques used to
Page 4-14
Mud
Bucket
Auger
Dutch
Auger
In situ Soil
Recovery
Auger
Eijkelcamp
Stony Soil
Auger
Planer
Auger
Applications
Limitations
Cohesive, soft or
hard soils, or
residues
General soil or
residue
Bit designed to
retain dry, loose,
or granular
material, silt,
sand, and gravel
Bit and bucket
designed to wet
silt and clay soil
or residue
Designed
specifically for
wet, fibrous, or
rooted soils
(marshes)
Collection of soil
sample in reusable liners;
closed top
reduces contamination from
caving sidewalls
Stony soils and
asphalt
Similar to
standard bucket
auger
Page 4-15
trating point is retracted and the sampler is advanced to collect the soil sample inside the removable tube. This sampler can reach depths of
30 60 feet or more in sand or fairly loose soil,
but has trouble penetrating clay and hard materials. As with any sampling device, hydraulic
rams have both advantages and disadvantages.
The advantages of direct-push technology include
the following:
Safety
Environmental
- If soil contamination is suspected,
large quantities of soil may have to be
put into containers such as drums and
stored or disposed of as hazardous
waste
- If the pit is refilled with excavated
soil, contaminated surface material
may be buried to a greater depth, or
contaminated soil from subsurface
layers may be exposed on the surface.
4.6.3.
Subsurface Geological/Geotechnical
Characterization
There are several drilling techniques that can be
utilized to characterize the subsurface geology of
a site. These drilling techniques do not provide
undisturbed soil samples and should not be used
in place of sonic drilling or cable tool methods.
4.6.3.1. Direct Mud Rotary
The direct mud rotary technique provides a flexible and rapid drilling method for a wide range of
borehole diameters in consolidated and unconsolidated materials. Direct mud rotary drilling uses
a rotating drill pipe with a hard-tooled drill bit
Page 4-18
5. Record the length of the tube used to penetrate the material being sampled and the number of blows required to obtain this depth.
6. Withdraw the sampler, and open it by unscrewing the bit and head and splitting the
barrel. The amount of recovery and the soil
type should be recorded.
Soil Probe
Shelby
Tubes
Soil
Recovery
Probe
Veihmeyer
Peat
Sampler
Applications
Disturbed
samples from
cohesive soil
Cohesive, soft
soils or residue;
representative
sample in soft to
medium cohesive soils and silts
Cohesive, soft
soils or residue;
special tips for
wet or dry soils
are available
Similar to thinwalled tube;
cores are collected in reusable
liners, minimizing contact
with the air
Cohesive soils or
residue to depth
of 3 meters
Limitations
Ineffective in
cohesionless sands;
not suitable for
collection of
samples for
laboratory tests
requiring
undisturbed soil
Sampling depth
generally limited to
less than one meter
Similar to
Veihmeyer tube
Similar to
Veihmeyer tube
Difficult to drive
into dense or hard
material; will not
retain dry, loose or
granular material;
may be difficult to
pull from the
ground
Wet, fibrous
organic soils
Page 4-21
Page 4-22
Page 4-23
useful for defining the boring depth where discrete soil samples should be collected for laboratory analysis. Soil recovery probes with dedicated or reusable liners (see Table 4-2) will minimize contact of the sample with the atmosphere.
Sampling Procedures
Low-Concentration VOC Soil Samples
Steps 1 5 are performed prior to transporting
VOC vials to the field for sample collection.
1. Add approximately 1 gram of sodium bisulfate to each vial. If samples that are markedly
smaller or larger than 5 grams are to be collected, adjust the amount of preservative to
correspond to approximately 0.2 grams of
preservative for each gram of sample.
Enough sodium bisulfate should be present to
ensure a sample pH of 2.
2. Add 5 milliliters of organic-free reagent water
to each vial. The water and the preservative
will form an acid solution that will reduce or
eliminate the majority of the biological activity in the sample, thereby preventing biodegradation of the VOAs.
3. Seal the vial with the screw cap and septum
seal. If double-ended, fritted vials are used,
seal both ends as recommended by the manufacturer.
4. Affix a label to each vial to eliminate the need
to label the vials in the field. This will ensure
that the tare weight of the vial includes the label. The weight of markings added to the label in the field is negligible.
Page 4-25
4.7.4.2. Sieving
Sieving eliminates large rock fragments. Under
some EPA protocols, only fine soil material
should be analyzed; see Figure 4-5 for an illustration of sieves.
Note: Do not sieve soil samples that are to be tested for
volatile organics.
Page 4-29
4.9.1.
Solutions
- Non-phosphate detergent
- Selected solvents such as acetone,
hexane, nitric acid, and isopropyl
alcohol
- Dilute bases
- Tap water
- Distilled or deionized water.
Tools and Supplies
- Long and short handled brushes
- Bottle brushes
- Drop cloth or plastic sheeting
- Paper towels
- Plastic or galvanized tubs or buckets
- Pressurized water sprayers
- Solvent sprayers
- Aluminum foil
- Trash bags
- Trash containers
- 55-gallon drums
- Metal or plastic buckets or containers
for storage and disposal of
decontamination solutions.
Solvent Rinses
- 10% nitric acid is typically used for
inorganic compounds such as metals.
An acid rinse may not be required if
inorganics are not a contaminant of
concern.
Chapter 4 Soil Sampling
Dilute
Acids
Dilute
Bases
Organic
Solvents2
Examples of
Solvents
Deionized water,
tap water.
Soluble
Contaminants
Low-chain hydrocarbons, inorganic
compounds, salts,
some organic
acids, and other
polar compounds.
Nitric acid Acetic Basic (caustic)
acid, boric acid.
compounds (e.g.,
amines and
hydrazines).
Sodium bicarboAcidic comnate (e.g., soap
pounds, phenol,
detergent).
thiols, some nitro
and sulfonic
compounds.
Alcohols, ethers
Nonpolar comketones, aromatics, pounds (e.g., some
straight-chain alka- organic comlines (e.g., hexane), pounds).
common petroleum
products (e.g., fuel,
oil, kerosene).
Hexane
PCBs
Organic
Solvents2
1
Material Safety Data Sheets (MSDSs) are required for all
decontamination solvents or solutions as required by the
Hazard Communication Standard.
2
4.9.2. Procedure
The following procedures should be used to clean
field sampling equipment between samples. Note
Page 4-30
Page 4-31
Equipment Rinse
- Fill a wash basin, a large bucket, or
childs swimming pool with tap
water. Approximately 10 50 gallons
of water may be required initially
depending upon the amount of
equipment to decontaminate and the
amount of gross contamination.
- Rinse soap off equipment with water
by immersing the equipment while
brushing. Repeat as many times as
necessary.
Low-Pressure Rinse
- Fill a low-pressure sprayer with
distilled or deionized water during the
rinsing process. Approximately 10
20 gallons of water may be required
initially depending upon the amount of
equipment to decontaminate and the
amount of gross contamination.
- Rinse sampling equipment with
distilled or deionized water with a
low-pressure sprayer.
Page 4-33
1 ASTM D5314 Standard Guide for Soil Gas Monitoring in the Vadose Zone2 California
Environmental Protection Agency, Department of Toxic Substances Control, Advisory Active Soil
Gas Investigation, April 2012,
http://www.dtsc.ca.gov/SiteCleanup/upload/VI_ActiveSoilGasAdvisory_FINAL_043012.pdf
3 DoD Vapor Intrusion Handbook, http://www.clu-in.org/download/char/dodvihdbk200901.pdf
4 USACE Sample Collection and Preparation Strategies for Volatile Organic Compounds in Solids,
October 1998
Page 4-34
Page 5-2
Page 5-3
Review Site
History
Source of Information
Activity
Groundwater Data, as
appropriate to the site
Sediment Data
Identify Site
Transport
Processes
Potential Sediment
Hydraulics
Assess wave/current-induced
resuspension, as appropriate to Redeposition of contaminated sediment
the site
Assess boat propeller wash,
as appropriate to the site
Page 5-4
Source of Information
Activity
Human Health-based
information
Water analysis for COPCs, partitioning variables (e.g., Octanol-Water Partition Coefficient (Kow)), oral dose
Evaluate receptor and exposure
In-vitro/in-vivo testing for bioavailability (e.g.,
pathways:
swine oral and dermal dose models); bulk
Direct contact
sediment analysis, partitioning measures ,
Ingestion
Tissue residue(s), fraction of COPC available
for uptake (bioaccessibility),
Identification of ingestion rates
Evaluate
Ecological and
Human Health
Pathways and
Endpoints
Page 5-5
or anthropogenically-affected reference). In
most DoD site investigations, the latter is desired;
in some state programs, the former is mandated.
To assure that grain-size, TOC, and eH conditions
are comparable may require sampling several
stations to achieve an acceptable match. Performance criteria for reference stations should be
included in project plans. Sampling intensity at
the reference station should also be sufficient to
establish a statistically valid comparison between
it and the investigation site.
Advanced methods to determine whether receptors are likely to show adverse effects, or to
elucidate release patterns and refine the CSM
with regard to contaminant mobility and bioavailability may also be included in a second or contingent phase of the investigation. Examples
include bedded sediment bioaccumulation testing,
collection of field organisms for tissue analysis,
measures of pore water, or benthic mapping
(section 5.8).
US EPA QA/G-5s
(http://www.epa.gov/quality/qs-docs/g5sfinal.pdf) provides useful guidance on statistical
sample design including numbers and types of
samples, selection of sample locations, sampling
frequency, and sampling and analytical protocols.
In addition, there are free software programs
available such as ProUCL and Visual Sample
Plan that permit estimation of numbers of samples required.
The analyte list for sediment and pore water
sampling schema should anticipate the intended
data uses. For instance, for toxicity testing, grainsize and total organic carbon are recommended;
for some analytes (e.g., organotins), bulk sediment may not be an appropriate medium and
pore-water analysis may be required. Some
analytes (e.g., mercury) have a short holding
time, which may affect the field schedule for
delivery to analytical laboratories. There are also
limitations on holding time for sediment prior to
initiating biological testing. The sampling method
and organism size to be retained from macro
invertebrate surveys should anticipate the uses of
data (e.g., taxonomic composition and mass,
species diversity measures).
Page 5-6
Water depth
- In less than 4 m of water, with low current
conditions and smooth water, the Birge-Ekman,
petite Ponar, Ponar, Van Veen, and Peterson
mini-Shipek grabs are recommended
- For deeper waters or greater current, the Ponar or Van Veen are recommended.
Sub-sampling from sampler directly
- If sub-sampling from the sampler is desired,
the Birge-Ekman, mini-Ponar, Ponar, Van
Veen, or Shipek are recommended
- If not, a Peterson, Smith-MacIntyre, or miniShipek are recommended.
Target sample depths
- Up to about 10 cm sample depth, a BirgeEkman, Ponar, or Shipek or miniature versions of any of these are suitable
- Up to about 30 cm, a Smith MacIntyre, Van
Veen, or Petersen grabs are suitable.
Target sample volumes to meet analytical
requirements
Page 5-7
- Up to about 3 L, the mini Birge-Ekman, petite Ponar, or mini-Shipek samplers are suitable
- 3 10 L samples may be collected with the
Birge-Ekman, Ponar, or Petersen grabs
- Above 10 L, Smith-MacIntyre or Van Veen
grabs are suitable.
For Sediment Grab Samples to be Subsampled in the Laboratory. The sample should
be transferred carefully and directly into a labeled container that is made of a chemically
inert material, tightly sealed, and air excluded.
For Sediment Grab Samples to be Subsampled in the Field. Typically, the sediment is
decanted into a cleaned bowl or bag for homogenization and sub-sampling. To minimize sediment handling and artifacts of sampling for
volatiles, samples may be taken directly from
the grab.
5.5.2. Sediment Core Sampling Methods
Core samplers (corers) are used to characterize
contamination over a depth interval that includes
sub-surface sediments. They also are used to
obtain sediment samples for geological characterizations and dating, investigate the historical
input of contaminants to aquatic systems, and to
characterize the depth of contamination at a site.
Corers are an essential tool for developing threedimensional maps of sediment contamination.
Collection of subsurface layers in addition to the
Chapter 5 Aquatic Sediment Sampling
For more information on methods for bulk sediment sampling, consult the following references:
Methods for Collection, Storage and Manipulation of Sediments for Chemical and Toxicological Analyses: Technical Manual (Ref. 1)
Sampling for Contaminants In Sediments and
Sediment Porewater (Ref. 6)
A Compendium of Chemical, Physical and
Biological Methods for Assessing and Monitoring the Remediation of Contaminated Sediment Sites (Ref. 7)
Ocean Testing Manual Evaluation of Dredged
Material Proposed for Ocean Disposal (Ref.
8)
Inland Testing Manual: Evaluation of
Dredged Material Proposed for Discharge in
Waters of the U.S. (Ref. 9).
Page 5-9
let light may be needed to assure the representativeness of sediment Polycyclic aromatic hydroChapter 5 Aquatic Sediment Sampling
Page 5-10
Organic sorbents are designed to reach equilibrium with the freely dissolved contaminant
phase in adjacent water. Quantitative results
can be obtained because the sorbent typically
has a known equilibrium coefficient that has
been derived from laboratory calibration studies using representative compounds. Additionally, higher concentrations of contaminants
occur in the sorbent, resulting in higher sensitivity than direct porewater measurements.
The period of exposure to assure steady state
depends upon the sorbent-water partitioning
coefficient and volume of sorbent exposed to
the pore water. High sorbent-water coefficients and large volumes of sorbent take longer
for hydrophobic contaminants to equilibrate.
Assurance or adjustments for steady state may
be assessed (in order of preference) by loss of
reference compounds with known characteristics that were introduced into the sorbent prior
to placement, selection of appropriate sorbent
thickness (hence volume), or by modeling contaminant transport into the sorbent.
An advantage of some samplers is that a single
device placed vertically in sediment can be
subdivided into sectors that may be separately
analyzed to generate a concentration profile.
This use of a sorbent sampler is useful in
monitoring the effectiveness of a sediment cap.
The gradient of concentrations that occur can
be further interpreted using advective flow
modeling.
Another advantage of sorbent samplers is that
they equilibrate with truly dissolved portion of
contaminants in water, hence do not measure
colloidally-bound contaminants, do not require
measurement of dissolved organic carbon to
substantiate equilibrium partitioning calculations, and generally do not require analytical
cleanup.
Chapter 5 Aquatic Sediment Sampling
Note: Analytical cleanup may be required for sulfur compounds that interfere with PCB analysis.
lengths of interest, and transferred to autosampling vials with a small volume of solvent
(e.g., 100 L), typically hexane or acetonitrile.
There are several commercially available
SPME sizes consisting of varying core size
and PDMS content in the coating. Those with
a 1000-m core are sturdy and resilient for
field use; those with a 210 m core are
somewhat less sturdy and harder to process in
the field into autosampler vials. Sorbent coats
with 30-m layers of PDMS are high capacity
and have slower uptake kinetics. A good
compromise between quick uptake kinetics
and ease of use and processing in the field is a
15 m PDMS layer on 1000 m core.
Note: Steady-state corrections are required for PCB congeners with Log Kows 6.
Page 5-15
Birge-Ekman, Van Veen, Ponar, and SmithMcIntyre grabs are often selected for infauna
in soft substrates (river backwaters, lakes, and
low-current velocity marine/estuarine conditions). Table 5-3 below summarizes characteristics of grab samplers.
Core samplers may be used, but they sample a
very small area and volume of sediment, thus
representativeness of the community may be
insufficient; however, this depends upon the
abundance of the community, and multiple
cores may be composited to provide sufficient
area/volume. See Table 5-4 below for comparison of coring methods.
For harder substrates and particularly for
epifaunal invertebrates, seines and trawls may
be used; however, seines and trawls typically
only gather larger organisms.
In flowing water, several techniques may be
used to harvest sediment-associated biota.
See Table 5-5 below for a summary of Stream
Net Samplers used to collect organisms from
flowing water.
Page 5-17
Device
Orange Peel
Use
Marine waters
and deep lakes
Sample
Depth
(cm)
Sample
Volume
(L3)
0 18
10 20
0 4 (in
deep sand)
10 20
Reasonable quantitative
samples
The trigger plates provide
added leverage essential to
its penetration of substrate
Advantages
Disadvantages
Birge-Ekman,
small
Lakes and
marine areas;
soft sediments,
silt, and sand
0 10
3.4
Birge-Ekman,
large
Lakes and
marine areas;
soft sediments,
silt, and sand
0 30
13.3
0 10
7.25
Ponar, petite
0 10
1.0
Deep lakes,
rivers, and
estuaries; useful
on sand, silt, or
clay
Page 5-18
Sample
Volume
(L3)
0 30
18 75
Adequate on most substrates May not close completethat are not compacted
ly, resulting in sample
Large sample obtained
loss
May close prematurely in
intact, permitting subrough waters
sampling
Available in stainless steel Metal frame may contaminate sample
Heavy, requires winch
Modified
Lakes and
Van Veen (e.g., marine areas
Ted Young
Grab)
0 15
18.0
Petersen
0 30
9.45
0 10
3.0
Shipek, mini
03
0.5
Device
Van Veen
Use
Deep lakes,
rivers, and
estuaries; useful
on sand, silt, or
clay; effective in
marine environments in deep
water and strong
currents
Deep lakes,
rivers, and
estuaries; useful
on most substrates
Advantages
Disadvantages
Page 5-19
Use
Sample
Depth
(cm)
Sample
Volume (L3)
Advantages
Disadvantages
Fluorocarbon
plastic or glass
tube (3.5 7.5 cm
inner diameter
(I.D.); 120 cm
long)
0 10
Same as above
except more
consolidated
sediments can
be obtained
0 10
0.96 0.44
Box corer
Same as above
but the depth of
the unconsolidated
sediment must
be at least 1 m
0 70
30.0
Difficult to handle
Relatively heavy, requiring larger vessel and power winch to deploy
Gravity corer,
Phlegar Corer (3.5
cm I.D., 50 cm
long)
0 50
0.48
Gravity corer,
Kajak-Brinkhurst
Corer (5 cm I.D.,
70 cm long)
0 70
1.37
03m
10.26
Benthos gravity
Soft, finecorer (6.6, 7.1 cm grained sediI.D., 3 m long)
ments
Page 5-20
Use
Alpine gravity
Soft, finecorer (3.5 cm I.D.) grained semiconsolidated
substrates
Piston corers
BMH-53 piston
corer
Waters 2 m
deep with
extension rod;
soft deposits
Boomerang corer
(6.7 cm I.D.)
Vibracorer
Continental
(5.0 7.5 cm I.D.) shelf of oceans,
large lakes;
sand, silty sand,
gravelly sand
substrates
Sample
Depth
(cm)
Sample
Volume (L3)
2m
Advantages
Disadvantages
1.92
3 20 m
5 40
2m
1m
3.52
36m
Labor intensive
Assembly and disassembly
might require divers
Disturbs surface
(0 0.5 m) layer
Special generator may be
needed
Heavier models require
larger boat and power
winch to deploy
Page 5-21
Table 5-5. A Summary of Stream Net Samplers Used to Collect Organisms from Flowing Water
Net Sampler
Habitats and
Substrates
Effectiveness of
Device
Advantages
Limitations
Surber Stream
Bottom Sampler
Shallow, flowing
streams, less than
32 cm in depth
with good current;
rubble substrate,
mud, sand, and
gravel
Performance
depends on
current and
substrate
Encloses area
sampled; easily
transported or
constructed; samples a unit area
Difficult to set in
some substrate
types, that is large
rubble; cannot be
used efficiently in
still, slow-moving
streams
Same as Surber
Same as Surber
Same as Surber
except completely
enclosed with
stable platform; can
be used in weed
beds
Same as Surber
Hess Sampler
Same as Surber
Same as Surber
Same as Surber
except completely
enclosed with
stable platform; can
be used in weed
beds
Same as Surber
Hess Stream
Bottom Sampler
Same as Surber
Same as Surber
Same as Surber
except completely
enclosed with
stable platform; can
be used in weed
beds
Same as Surber
Stream-bed Fauna
Sampler
Same as Surber
Same as Surber
Same as Surber
except completely
enclosed with
stable platform; can
be used in weed
beds
Same as Surber
Drift Nets
Flowing rivers
and streams; all
substrate types
Effective in
collecting all
taxa which drift
in the water
column
Low sampling
error; less time,
money, and effort;
collects macroinvertebrates from all
substrates; usually
collects more taxa
Unknown where
organisms come
from; terrestrial
species may make
up a large part of a
sample in summer
and periods of wind
and rain; does not
collect non-drifting
organisms
Page 5-22
tion of benthic data and contaminant concentrations. The benthic habitat may need to be monitored over time to determine the effects of habitat
change due to natural or human impacts, and to
assure effective implementation of remediation
strategies.
5.8.2.
Page 5-25
5.9. References
1
Measurement and Monitoring Technologies for the 21st Century, Sampling for Contaminants
In Sediments and Sediment Pore Water (http://clu-in.org/programs/21m2/sediment/)
EPA Handbook, A Compendium of Chemical, Physical and Biological Methods for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
(http://www.epa.gov/eerd/methods/108Complete.pdf)
10
11
ITRC 2011, Incorporating Bioavailability Considerations into the Evaluation and Remediation of Contaminated Sediment Sites (http://www.itrcweb.org/contseds-bioavailability)
12
EPA-905-B94-002, Assessment and Remediation of Contaminated Sediments (ARCS) Program - Assessment Guidance (http://www.epa.gov/glnpo/arcs/EPA-905-B94-002/EPA-905B94-002.html)
13
ASTM E1391, Standard Guide for Storage, Characterization, and Manipulation of Sediments for Toxicological Testing and for Selection of Samplers Used to Collect Benthic Invertebrates
14
Page 5-26
15
ASTM D4823, Standard Guide for Core Sampling Submerged, Unconsolidated Sediments
16
ASTM D4387, Standard Guide for Selecting Grab Sampling Devices for Collecting Benthic
Macroinvertebrates
17
Mudroch, A. and S. MacKnight, (Eds). 1994. Handbook of Techniques for Aquatic Sediments Sampling, Second Edition, Lewis Publishers, Boca Raton, FL.
18
Mudroch, A. and J. Azcue, 1995. Manual of Aquatic Sediment Sampling. Lewis Publishers,
Boca Raton, FL.
19
ASTM D3976, Standard Practice for Preparation of Sediment Samples for Chemical Analysis
20
ASTM E1367, Standard Test Method for Measuring the Toxicity of Sediment-Associated
Contaminants with Estuarine and Marine Invertebrates
21
ASTM E729, Standard Guide for Conducting Acute Toxicity Tests on Test Materials with
Fishes, Macroinvertebrates, and Amphibians
22
NFESC Technical Report 1902, Coastal Contaminant Migration Monitoring: The Trident
Probe and UltraSeep System: Hardware Description, Protocols, and Procedure
(http://www.spawar.navy.mil/sti/publications/pubs/tr/1902/tr1902cond.pdf)
23
NFESC Technical Report 1966, Monitoring of Water and Contaminant Migration at the
GroundwaterSurface Water Interface
(http://www.spawar.navy.mil/sti/publications/pubs/tr/1966/tr1966cond.pdf)
24
ASTM E1706, Standard Test Method for Measuring the Toxicity of Sediment-Associated
Contaminants with Freshwater Invertebrates
25
ASTM E1611, Standard Guide for Conducting Sediment Toxicity Tests with Polychaetous
Annelids
26
27
28
EPA-841-B-99-002, Rapid Bioassessment Protocols for Use in Streams and Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish - Second Edition
(http://water.epa.gov/scitech/monitoring/rsl/bioassessment/index.cfm)
29
EPA/R-99/064, Methods for Measuring the Toxicity and Bioaccumulation of Sedimentassociated Contaminants with Freshwater Invertebrates - Second Edition
(http://water.epa.gov/polwaste/sediments/cs/upload/freshmanual.pdf)
30
EPA/600/R-01/020, Methods for Assessing the Chronic Toxicity of Marine and Estuarine
Sediment-associated Contaminants with the Amphipod Leptocheirus Plumulosus
(https://www.clu-in.org/download/contaminantfocus/sediments/leptocheirusj.pdf)
31
EPA/600/R-01/108, Comparisons of Boating and Wading Methods Used to Assess the Status
of Flowing Waters (http://www.epa.gov/eerd//methods/MCD_nocover.pdf)
Page 5-27
32
Page 5-28
6.5.1.
Representative Sampling
Considerations
To collect a representative sample, the hydrology,
shape, and size of an impoundment should be
determined prior to sampling. This will aid in
determining the presence of phases or layers in
lagoons, flow patterns in streams, and appropriate
sample locations and depths.
Page 6-3
Page 6-4
Page 6-8
Page 6-9
Page 6-10
Page 6-12
Advantages
Disadvantages
Difficult to label wet
bottle.
Pre-preserved bottles
cannot be used.
Exterior of bottle may
contact the sample.
Pond
Sampler
Weighted
Bottle
Sampler
Can be fabricated or
purchased.
Remains unopened
until it reaches
sample depth.
Wheaton
Dip
Sampler
Allows discrete
Sampling depth is limited
samples to be taken at by the length of the
depth.
poles.
Exterior of bottle may
contact the sample.
Kemmerer
Depth
Sampler
Ability to sample at
Sampling tube is exposed
various and great
to water while traveling
depths.
down to sampling depth.
Allows discrete
samples to be taken at
depth.
Bacon
Bomb
Sampler
Allows discrete
Difficult to
samples to be taken at decontaminate.
If brass construction,
depth.
may not be appropriate in
metals analysis or
toxicity testing.
Difficult to transfer
sample to container.
The sample can become
aerated.
PACS
Grab
Sampler
Allows discrete
Depth of the sampling is
samples to be taken at limited by the length of
depth.
the pole.
Difficult to
decontaminate.
Point
Source
Bailer
Allows discrete
May be difficult to
samples to be taken at operate.
Difficult to
depth.
decontaminate.
Automated
Sampler
Allows discrete
Not appropriate for
samples to be taken at collecting samples
depth.
requiring VOC and
microbiological analysis.
May be incompatible
with some liquids.
Laboratory-supplied
bottle may not fit into the
sampler.
Mixing of the sample
may occur.
Page 6-13
Page 6-14
Sampling requirements
The outfalls to be monitored
Chapter 7 Storm Water Sampling
Page 7-2
Page 7-3
All other discharges associated with the construction activity are prohibited by the CGP and
will require coverage under an individual storm
water permit or another type of NPDES permit.
7.3. Storm Water Compliance
The intent of the Phase I and Phase II regulations
are to prevent storm water from becoming contaminated by industrial or construction activities,
rather than requiring quantitative monitoring of
storm water outfalls. To implement the intent of
the regulation, the control authority (EPA or the
state) requires a systematic approach be taken to
identify the facilitys potential storm water
impacts, and to mitigate these impacts through a
series of best management practices (BMPs).
BMPs can be either non-structural or structural.
Non-structural BMPs include procedural
changes such as not allowing off-loading of fuel
during rain events, covering of storm-drains
during material transfer, or not storing materials
outside. Structural BMPs are physical changes
to the facility or implementation of technologies
to prevent pollutants from leaving an industrial
Page 7-4
Page 7-5
Table 7-1 lists some of the industrial-type activities common at DoD facilities that may require
Phase I Industrial
Classification
Additional
SWPPP Reqs.b
Chemical
Samplinga
Table 7-1. Potential Industrial Activities at DoD Installations with Storm Water Considerations
Motor Pools
Yes No
Airfields
Yes Yes
Wastewater Treatment
Plants
(iv) Hazardous waste. Only if Sector K. Only if the installation has a RCRA
RCRA permitted facility.
permit.
Department of Logistics
Terminals/ Loading Facilities
(i) Facilities subject to effluent Sector AA. Produces plated ware or fabricated
metal products, except for electrical-related,
limitation guidelines.
machinery, and transportation equipment.
Yes Yes
Ammunition/Ordnance
Production Operations
Yes Yes
No Yes
No Yes
Sector AC.
No
None.
Yes No
Yes No
No
No
Yes Yes
No
Page 7-7
Phase I Industrial
Classification
Additional
SWPPP Reqs.b
Chemical
Samplinga
Yes Yes
Sector X.
No Yes
None.
N/A N/A
Industrial facilities with a general permit or individual permit that requires compliance sampling
are usually required to collect and analyze a grab
sample taken within the first 30 minutes of a storm
event and flow-weighted composite samples from
each of the industrial storm water point source
outfalls identified in the Storm Water Pollution
Prevention Plan (SWPPP). If possible, all outfalls
should be sampled during the same representative
storm event. The descriptions of each storm event
and the outfalls sampled must be recorded.
Page 7-10
Date of Inspection:
End Date of last rain event:
Inspector name:
Type of outfall
Concrete Pipe
Grassed
Rock
Other
6.
Page 7-11
Problem:
Solution:
Problem:
Solution:
Problem:
Solution:
Problem:
Solution:
Problem:
Solution:
Sampling in manholes.
Sample in manholes only when necessary, as
this requires training on confined space entry.
Problem:
Solution:
7.5.3.
Page 7-13
Table 7-2. Typical Storm Water Pollutants, Possible Analytical Methods, and Sample Collection
Techniques
Storm Water Pollutant
pH
Temperature
Oil and Grease
TSS
BOD5
COD
Nitrate and Nitrite Nitrogen
Ammonia Nitrogen
Fecal Coliform
Fecal Streptococcus
Total Phosphorous
Priority Metals
Total Cyanide
Total Phenolics
VOCs
SVOCs
Pesticides
Sample Technique
Grab
Grab
Grab
Flow-Weighted Composite
Flow-Weighted Composite
Flow-Weighted Composite
Flow-Weighted Composite
Flow-Weighted Composite
Grab
Grab
Flow-Weighted Composite
Flow-Weighted Composite
Flow-Weighted Composite
Flow-Weighted Composite
Grab
Flow-Weighted Composite
Flow-Weighted Composite
Table 7-3. Comparison of Manual and Automatic Sampling Techniques for Collection of
Storm Water Samples
Sampling Technique
Manual Grabs
Advantages
Appropriate for all pollutants
Minimum equipment required
Disadvantages
Labor intensive
Environment possibly dangerous to field personnel
May be difficult to get personnel and equipment to
the storm water outfall within the 30 minute
requirement
Potential for human error
Manual
Flow-Weighted
Composites (multiple grabs)
Labor-intensive
Environment possibly dangerous to field personnel
Human error may have significant impact on
sample representativeness
Requires flow measurements taken during sampling
Automatic Grab
Samplers
Page 7-14
Sampling Technique
Advantages
Automatic
Flow-Weighted
Composite Samplers
Disadvantages
Cross-contamination of aliquot if tubing/bottles
not properly washed
Not acceptable for VOCs sampling
Costly if numerous sampling sites require the
purchase of equipment
Requires equipment installation and maintenance,
may malfunction
Requires initial operator training
Requires accurate flow measurement equipment
tied to sampler
Cross-contamination of aliquot if tubing and
bottles not properly washed
V-Notch
(90)
(60)
(45)
(30)
(22)
Q = Flow Rate
(1 inch)
(2 inches)
(3 inches)
(6 inches)
(9 inches)
(1-8 feet)
(10-50 feet)
Flow
Top View
W
Q = 3.33 L H1.5
Throat
Converging
Section
Side wall
Diverging
Section
A
Side View
L
H
Contracted
Q = 3.367 b H1.5
Cipolleti (trapezoidal)
Source: Civil Engineering Reference Manual. 5th Edition, by Michael R. Lindeburg, PE,
with permission from the publisher, Professional Publications, Inc.,
Belmont, California, 1989.
Brace
B
Flow
A
PLAN
Trim to fit
As required
Palmer-Bowlus
Flow
Source: Wastewater Engineering: Treatment, Disposal, Reuse. 2nd Edition, Metcalf &
Eddy, Inc., with permission from the publisher, McGraw-Hill Book Co., New York, 1979.
Page 7-16
7.7.1.
The frequency of sampling for non-visible pollutants must be determined based on the exposure
of pollutant sources. Runoff only needs to be
sampled when there is exposure of a pollutant
source to storm water that enters a storm drain or
surface water. Inspections of material storage
areas that identify a non-structural or structural
BMP failure that exposes potential non-visible
pollutants to storm water that runs off the construction site will trigger a requirement for sampling and analysis. If spills are cleaned up and
the contaminated material is isolated, eliminating
exposure to storm water runoff, then sampling is
not necessary. For instances when the potential
for previously existing contamination is identified, it may be appropriate to conduct screening
analysis during the first one or two storm events
of the season to determine if the potential contaminant is running off the construction site. Figure 7-7 provides a flow chart to help determine
when sampling and analysis is required.
7.7.3.
Page 7-18
affected by material storage, historic contamination or other exposed potential pollutants, and the
background runoff quality (i.e., uncontaminated
sample). Material storage may be confined to a
small area of the project site while historic contamination or exposed materials such as soil
amendments, may be widely spread throughout
the construction site. For this reason, the sampling locations identified for these two types of
potential pollutants may be different.
Samples must be collected at locations identified
in the SWPPP or areas identified by visual observations or inspections where there has been a
structural BMP failure or breach that can be
safely accessed. A location that is not affected by
material storage activities or by runoff from
material storage areas should be selected as a
background or reference sampling location for
collecting the uncontaminated runoff sample. For
a widely spread potential contaminant, sampling
locations may need to be selected at the perimeter
of the site, where storm water enters (unaffected
by site activities) and leaves (affected by site
activities).
7.7.5.
Page 7-19
Potential Pollutant
Source
Field Indicator of
Pollutant Release
Laboratory Analysis
Line Flushing
Chlorinated water
Colorimetric kit
Residual chlorine
Portable Toilets
Bacteria, disinfectants
N/A
Total/fecal coliform
Concrete &
Masonry
Acid wash
pH meter
pH
Curing compounds
pH meter
pH meter
pH
Resins
N/A
SVOCs
Thinners
N/A
VOCs
Paint strippers
N/A
VOCs
Solvents
N/A
VOCs
Adhesives
Phenols kit
Phenols, SVOCs
Sealants
N/A
SVOCs
Detergents
Colorimetric kit
Surfactants, phosphates
Bleaches
Colorimetric kit
Residual chlorine
Solvents
N/A
VOCs
Pesticides/herbicides
N/A
Fertilizers
N/A
pH meter
Acidity/alkalinity
Aluminum sulfate,
sulfur
pH meter
TDS, alkalinity
Treated Wood
Copper, arsenic,
selenium
Metals
Soil Amendments
& Dust Control
Lime, gypsum
pH meter
pH
Plant gums
N/A
BOD
Magnesium chloride
N/A
Alkalinity, TDS
Calcium chloride
N/A
Alkalinity, TDS
Natural brines
N/A
Alkalinity, TDS
Lignosulfonates
N/A
Alkalinity, TDS
Painting
Cleaning
Landscaping
Page 7-20
Figure 7-7. Decision Diagram to Determine When Construction Storm Water Sampling is
Necessary
Start
Prepare SWPPP
Are there
pollutants present that
are not visually
detectable in storm
water discharge?
No
Yes
No sampling and
analysis required for
these pollutants
No
Is pollutant
stored in a water tight
container in a building
or under a water tight
roof?
Yes
Does visual
monitoring indicate
breach, malfunction,
leakage, or a spill, resulting in
release of pollutant so that it
could be discharged
in storm water
runoff?
No
Yes
Page 7-21
7.7.6.
Page 7-22
Sampling SOP
FLB/FN
Pen(s)
Containers
Preservatives
Labels
Markers
Coolers
Ice
Packing Material
Packaging Tape
COC form
Custody seals (if required)
Decontamination storage containers,
equipment, and materials
Personal safety equipment, safety test
equipment
Field screening or testing equipment,
standards, reagents, and SOP
Testing Field Forms or Logbooks.
Page 7-24
8.2. Scope
Groundwater monitoring wells, underground
injection wells, and industrial wells are the potential sources of groundwater samples. This chapter includes the minimum criteria to be followed
to obtain representative samples. Variations from
these criteria should be necessary only when
required by regulatory practices (e.g., statespecific requirements) or site historical data
gathering practices. Analytical data derived from
samples obtained in a way that does not follow
the documented sampling plan should not be
accepted. For construction and design of
groundwater monitoring wells, refer to ASTM
D5092-04, Standard Practice for Design and
Installation of Groundwater Monitoring Wells.
Figure 8-1 displays a diagram of a typical
groundwater monitoring well.
Figure 8-1. Diagram of a Typical Monitoring
Well
groundwater samples. The development of a sitespecific SAP is the first step toward collecting a
representative groundwater sample. Each SAP is
an instruction manual for field personnel and
should be built around the objectives and sampling strategy. See Chapter 2 for a detailed discussion of SAP development applicable to all
sampling programs. The discussion below focuses on SAP development for groundwater sampling programs specifically.
The SAP should consider a variety of factors,
including site hydrogeology, the condition and
accessibility of monitoring wells, suspected
pollutants, DQOs, analytical methods and detection limits, the groundwater collection method,
sample handling procedures (e.g., filtration,
preservation requirements, COC), and safety.
The SAP cannot be implemented effectively if field
personnel do not understand its contents. Many
times the primary reason that groundwater sampling
events are problematic is that the person preparing
the SAP is not the person in the field. One method
that alleviates this problem is assigning a Sampling
Team Leader who is responsible for all activities in
the field. The Sampling Team Leader will work
closely with those individuals preparing the SAP to
understand fully the objectives of the project. The
Sampling Team Leader is responsible for all individuals in the field. If required, he or she also is
responsible for providing additional training to field
personnel before fieldwork begins.
8.3.3. QA
Groundwater monitoring programs encompass a
variety of information sources and include both
primary and secondary data collection. These
data sources are used to continuously update the
conceptual site model and allow Site Managers to
make decisions regarding further investigation,
additional monitoring, remediation alternatives,
or site closure.
The level of data quality for each groundwater
monitoring program, and many times for each
specific sampling event, depends on the intended
use of the data. For example, the level of QA/QC
needed for groundwater samples that are colChapter 8 Groundwater Sampling
Type of well
Depth of well
Diameter of well casing
Depth to water
Contaminants likely to be encountered
Analytes of interest
Length of open hole (bedrock well)
Type, slot size, and length of screen
Page 8-5
This section describes the procedures for sampling monitoring wells. It describes collection of
field measurements, well evacuation procedures,
and groundwater sampling procedures.
8.6.1.
Field Measurements
Page 8-7
Gallons/Linear foot
2 inch (0.1667)
0.1632
4 inch (0.3333)
0.6528
6 inch (0.5000)
1.4688
8 inch (0.6667)
2.6112
10 inch (0.8333)
4.0800
12 inch (1.0000)
5.8752
Example:
Total depth of well casing:
Depth to water:
Linear feet of water:
2-inch casing:
100 ft.
-20 ft.
80 ft.
x 0.1632
13 gal.
Before Purging
Date, time, and weather conditions
Well number and permit number
PID or FID reading taken from the well
immediately after the cap is removed
Presence and thickness of free product
pH, DO, temperature, and specific
conductivity
Total depth of well from the top of inner
casing or surveyors mark if present
Depth from the top of inner casing to the top of
screen
Depth from the top of inner casing to water
Estimated water volume in well.
After Purging
Start and end time purging
Purge method
Purge rate(s)
Total volume purged
pH, DO, temperature, and specific
conductivity.
After Sampling
Start and end time for sampling
pH, DO, temperature, and specific
conductivity
Sampling method.
Any field observations made during the groundwater sampling event (e.g., slow recharge, turbidity, odor, sheens, and PID or FID readings) also
should be reported.
Air-sensitive parameters such as DO, pH, temperature, and specific conductance are best analyzed with the use of a flow-through cell, eliminating sample exposure to air. However, monitoring of these air-sensitive parameters for well
It is important to ensure that the purging procedure or equipment does not cause crosscontamination from one well to the next. Therefore, the preferred method employs dedicated
tubing (new dedicated linear polyethylene ASTM
drinking water grade) and pumps. Because it
may not be practical to dedicate a pump to a
specific well, it is permissible to decontaminate
this equipment between wells. Methods for
decontamination should be specified in the sitespecific SAP.
Prior to purging, check the well for floating product. During purging, the pump intake or tubing
should be kept at a maximum distance of 6 feet
below the water level to prevent disturbance of
sediment on the bottom of the well. The pump
intake or tubing should be lowered as the water
level decreases to maintain this distance and
ensure sufficient distance from the air/water
interface. In instances where the total depth of
standing water in the well casing is less than 6
feet, begin purging near the top of the water
column and lower the tubing as stated above.
Following this procedure, Field Sampling Personnel should ensure that all static water is removed prior to sampling.
Page 8-10
rate must be low enough to minimize mobilization and entrainment of particulate matter that is
not mobile under non-pumping conditions. Typically, flow rates between 0.1 and 0.5 liters per
minute are used; however, the selection of an
appropriate flow rate is dependent on site-specific
hydrogeology. Water level drawdown provides
the best indication of the stress imparted by a
given flow rate for a given hydrological situation.
Measure the initial static water level, and then
monitor the water level of the well during purging
using either a continuous water-level measurement device such as a pressure transducer or
bubbler, or make periodic measurements (every 1
to 2 minutes) using an electric tape or similar
measuring device. If drawdown is rapid and
continuous, reduce the pumping rate until drawdown stabilizes. If drawdown is very slow or
imperceptible, the pumping rate can be increased.
When drawdown and water-quality indicator
parameters (e.g., conductivity, DO) have stabilized, sampling can begin in accordance with the
sites approved sampling and analysis plan.
In general, the advantages of low-flow purging
and sampling include the following:
More representative of the mobile load of
contaminants (dissolved and colloidassociated)
Minimal disturbance of the well, thereby
minimizing sampling artifacts
Less operator variability, and greater operator
control
Reduced stress on the formation (minimal
drawdown)
Less mixing of stagnant casing water with
formation water
Reduced need for filtration
Smaller purging volume, which decreases
waste disposal costs and sampling time
Better sample consistency, and reduced artificial sample variability.
Some disadvantages of low-flow purging include
the following:
Generally not suitable for use in low-yield
wells
Page 8-13
sampled. The preferred apparatus is a Tefloncoated stainless steel cable attached to a lowgear-ratio winch, which is connected to a tripod
standing over the well. This apparatus is preferred because it provides the most reproducible
bailing method. If this apparatus is not available,
the bailer may be lowered by hand using a Teflon-coated stainless steel leader.
Note: Braided stainless steel cable is coated with manufacturing oils that make decontamination difficult. Therefore,
Teflon coated, stainless steel is required for the bailer
leader since it will come into contact with the groundwater.
VOAs
Purgeable organic carbons
Purgeable organic halogens (POXs)
Total organic halogens (TOXs)
TOC
Base neutrals/acid extractables
Oil and grease/total petroleum hydrocarbons
(O&G/TPH)
8. PCBs/pesticides
9. Total metals
10. Dissolved metals
11. Phenols
12. Cyanide
13. Sulfate and chloride
14. Turbidity
15. Nitrate and ammonia
16. Preserved inorganics
17. Radionuclides
18. Non-preserved inorganics
19. Bacteria.
This collection order takes into consideration the
volatilization sensitivity of groundwater samples.
Additional information on the order of sample
collection can be found in RCRA and the
Groundwater Monitoring Technical Enforcement
Guidance Document, September 1986.
8.6.5.
Page 8-16
toward any zones of higher conductivity intersected by, or adjacent above or below the
screened interval. Also, flow induced by pumping, even at low-flow rates, can mobilize and
suspend solids that are immobile under ambient
laminar flow conditions in the aquifer, thereby
artificially elevating turbidity. This can result in
measured concentrations being affected by the
sampling process, particularly for metals. Vertical flow through the well caused by the screen
intersecting zones of different head also can bias
the representativeness of low-flow samples, as
well as that of passive samples, particularly if net
vertical flow through the well bore exceeds the
purge rate (sampled water will be biased toward
the source of flow). Side-by-side comparisons
and historical data show that concentration results
obtained by low-flow sampling most often are
very similar to concentration results obtained by
passive sampling (ITRC, 2007). Understanding
differences that may be observed often can provide valuable insight into contaminant distribution and hydrologic characteristics of a site.
8.6.5.2. Characteristics of Passive Samples
Passive samplers:
Page 8-17
groundwater. The appropriate period of deployment also considers the time required for well
flow dynamics and ambient conditions to restabilize from placement of the sampler or other
disturbance. The rule of thumb is that a 14-day
deployment period is ample for most types of
diffusion samplers, analytes, and hydrologic
conditions (ITRC, 2004; ITRC, 2007). Because
analytes always diffuse across the membrane
from higher to lower concentration, the samplers
maintain equilibrium concentrations and track
changes in concentration in the well water (within
the equilibration time lag period) regardless of
how long the sampler was deployed in the well.
The very small pore sizes of diffusion sampler
membrane materials eliminate turbidity, thus
diffusion samplers represent only the truly
aqueous (dissolved) concentrations of analytes.
Polyethylene Diffusion Bag (PDB) Sampler.
(Vroblesky and Hyde, 1997; Vroblesky, 2001;
ITRC, 2004) was the first diffusion sampler to
become widely known for sampling groundwater.
PDBs are constructed of low-density polyethylene tubing of 4 mil thickness, having a pore size
of about 10 angstroms. They are appropriate for
sampling only hydrophobic (low water solubility)
VOCs, chlorinated solvents, and short chain
aliphatic hydrocarbons (up to about C10). The
hydrophobic nature of the polyethylene membrane makes PDBs inappropriate to sample for
analytes that are highly soluble in water (e.g.,
ketones, alcohols, etc.) or dissolved ionic species
(e.g., metal cations, anions). Tables listing many
field- and laboratory-tested analytes are found in
Vroblesky (2001a), Vroblesky and Campbell
(2001), ITRC (2004), and ITRC (2006).
Regenerated Cellulose Dialysis Membrane
Sampler. (Imbrigiotta and others, 2007) is similar in concept to the PDB, but uses a hydrophilic
cellulose membrane. The dialysis membrane
sampler was developed and demonstrated by
researchers at the US Geological Survey (Ehlke
and others, 2004) to provide a passive diffusiontype sampler appropriate for inorganic as well as
organic analytes. It has been demonstrated as
suitable for sampling dissolved concentrations of
Page 8-18
sample collection. The sample is collected immediately prior to, or as a result of sampler retrieval. Properly collected whole-water grab
samples capture suspended particles that are
naturally mobile in the aquifer under ambient
laminar flow conditions, but do not have elevated
turbidity resulting from the sampling activity.
One of the more recently developed devices seals
the sample in situ at the sampling point in containers (e.g., 40-mL VOA vials or other containers) that can be placed directly into auto-samplers
at the laboratory, thus eliminating all exposure of
the sample to air or other influences. Sample
transfer can cause loss of VOC analytes, and
exposure to air can cause changes in oxidationreduction potential affecting redox-sensitive
metal concentrations.
Accumulationtype Samplers. Rely on both
diffusion and adsorption of analytes. Analytes
diffuse through a semi-permeable membrane and
are accumulated onto an adsorbent medium within the sampler. Both the diffusion membrane and
adsorbent material must be appropriate for the
analyte(s) of interest. The total analyte mass
accumulated on the adsorbent medium over the
entire deployment period is measured. Accumulation samplers have been used to sample surface
water (e.g., bioaccumulation studies) for several
decades (e.g., the SPMD, Polar Organic Chemical
Integrative Sampler (POCIS)) (ITRC, 2006;
Verreydt, 2010), and for air and soil vapor studies
(ITRC, 2006). More recently the methodology
has been applied to determine VOC concentrations in groundwater wells using the Gore
Module (ITRC, 2007). An average accumulation
rate over the deployment period is easily calculated, but estimates of concentration in the medium being sampled depend on a significant
number and range of analyte-specific, samplerspecific, and environmental variables (e.g., membrane and analyte diffusion properties, adsorbent
uptake rate, temperature, pressure, etc.). Proprietary empirical data for the Gore Module is used to
infer VOC concentrations in groundwater. Accumulation samplers have a particular advantage
in that the deployment period can be extended to
concentrate analyte mass and detect analytes
Page 8-19
Vroblesky, D.A. (2001a). Users Guide for Polyethylene-Based Passive Diffusion Bag Samplers
to Obtain Volatile Organic Compound Concentrations in Wells, Part 1: Deployment, Recovery,
Data Interpretation, and Quality Control and
Assurance, U.S. Geological Survey Water Resources Investigations Report 01-4060.
Vroblesky, D.A., 2001b, Users Guide for Polyethylene-Based Passive Diffusion Bag Samplers to
Obtain Volatile Organic Compound Concentrations in Wells, Part 2: Field Tests, U.S. Geological Survey Water Resources Investigations Report 01-4061.
Page 8-20
Sealed-screen samplers
Multi-level samplers (or vertical profilers)
Open-hole samplers.
With these tools, the time needed to retrieve the
sample will vary according to the hydraulic conductivity of the sampling zone. In general, sampling within coarse-grained sediments takes
minutes, while sampling within fine-grained
sediments can take several hours or more. In
situations where slow recharge inhibits the timely
collection of groundwater samples, the sampler
may be left in place to recharge while the DPT rig
is moved to a new sampling location.
8.7.2.1. Sealed-Screen Samplers
Sealed-screen samplers typically consist of a
short (6 inch 3-foot) screen nested within a
sealed, watertight tool body. Because the screen
is not exposed to the formation as the sampler is
advanced into the subsurface, the screen does not
become plugged or damaged. In addition, the
potential for cross-contamination is greatly reduced and a true depth-discrete sample that is
representative of the target sampling zone can be
collected. The sample volume collected with
some sealed-screen samplers is limited by the
volume of the sample chamber.
To collect the sample, the sealed-screen sampler
is advanced to the target sampling depth, and the
protective outer rod is retracted, exposing the
screen to groundwater. Groundwater flows
Page 8-21
Page 8-24
3.
4.
5.
6.
7.
8.
9.
8.8.7.
the well by setting the pump intake of the submersible or suction-lift pump several feet above
the DNAPL.
8.8.8.
This section provides a brief discussion on sampling industrial wells used to extract process
water and potable water. Site Managers should
always consult the state environmental agencies
drinking water division to determine specific
requirements.
- Peristaltic pump
- Air lift pump
- Bladder pump (gas squeeze pump)
- Packer pump
- Gas piston pump
- Gas displacement pump
- Inertial pump
Groundwater sampling equipment
- Passive diffusion bags for VOCs
- Bottom fill bailer (single or double check
valve)
- Peristaltic pump
- Bladder pump
- Packer pump
- Inertial pump
- Syringe sampler
Additional equipment
- VOCs detection devices, such as PID or
FID
- Appropriate hand tools
- Keys to locked wells
- Filtering devices
- Field measurement instrumentation
(e.g., temperature, specific conductance,
pH, DO, turbidity)
- Plastic sheeting
- Dedicated, pre-cleaned stainless steel
pitchers, or an equivalent dipping device
- Calibrated bucket for purged water
measurement
- Distilled or deionized water or ASTM Type
II water
- Laboratory-grade glassware, detergent, or
cleaning materials
- Empty drums for collection of purged water
- Stainless steel clamps.
Page 8-29
Page 8-30
Water source
Source vulnerability
Analyses to be performed
Chapter 9 Drinking Water Sampling
Regulatory requirements
DQOs
The population served
Anticipated or potential contaminants
System size.
9.4.2.
Site-Specific SAP
A site-specific SAP should be prepared and reviewed by appropriate regulatory personnel prior
to starting any sampling event to ensure the proper location, parameters, and number of samples
are taken to meet compliance requirements. The
specific monitoring and reporting requirements of
the SDWA are beyond the scope of this handbook.
The site-specific SAP is an instruction manual for
field personnel. It should be built around the
objectives and sampling strategy. The SAP must
consider a variety of factors including the water
source, condition and accessibility of sampling
locations, suspected contaminants, analytical
methods and detection limits, collection methods,
sample handling procedures, and safety. See
Chapter 2 for a detailed discussion of SAP development applicable to all sampling programs.
Note: Site-specific sampling requirements are unique, and
local, state, and federal regulatory authorities should be
consulted to ensure the drinking water sampling program is
adequately prepared.
Page 9-3
Page 9-4
Inorganic contaminants
Microbiological
Metals
SVOCs
DPBs
Radionuclides.
9.6.1.2. Sampling Procedures
The general procedure for collecting samples
from a tap includes the following steps:
1. Determine the appropriate sample location
and assemble all necessary materials. The
proper preservative should be added by the
laboratory or be available in the field for addition to the sample. A dechlorinating agent is
used when sampling chlorinated waters (such
as those found in the distribution system).
Handle the sterilized containers carefully to
avoid contamination.
2. Go to the sampling location(s) specified in the
SAP. Drinking water sampling locations are
usually located in the distribution system and
are accessible during the day. Examples include hospitals, city buildings, restaurants,
pump stations, and dedicated sampling stations. The tap should be clean and in good
condition (i.e., no leaks). To minimize contamination, avoid drinking fountains and faucets with swivel necks unless specific pointof-use concerns arise. If the sampling location does not have an accessible tap, then a
separate, clean, 1-liter plastic or glass (as appropriate) container should be used to dip and
Chapter 9 Drinking Water Sampling
20
0.2
.16
.82
30
0.3
0.4
1.2
40
0.4
0.9
1.6
50
0.5
1.1
2.0
100
1.0
2.3
4.1
Page 9-6
Page 9-7
Microbiological
Metals
SVOCs
Inorganic contaminants
Radionuclides.
9.6.4.2. Sampling Procedures
Refer to Chapter 6, Surface Water Sampling, for
further guidance and sampling procedures.
9.6.5. Source Water Sampling From a Well
Source water sampling from wells is appropriate
for most drinking water sampling parameters, as
it will determine the level of treatment required to
bring the water into compliance with federal,
state, and local statutes.
9.6.5.1. Appropriate Parameters
Source water sampling of wells is an acceptable
method for the following parameters:
Microbiological
Metals
SVOCs
Inorganic contaminants
Radionuclides.
9.6.5.2. Sampling Procedures
The general procedure for collecting source water
samples from wells is as follows:
Obtain as much information as possible from the
well owner, including depth of the well, well
yield, formation in which the well is completed,
screen depth and length, well construction material, diameter of casing and when and by whom
the well was installed. This information should
be verified if possible by obtaining drilling logs,
etc. With this information, the correct sampling
approach, as well as the number of gallons to be
evacuated, can be determined so that the collected
sample represents the condition of the groundwater.
For long-term monitoring projects utilizing domestic wells, a specific tap or faucet should be
Page 9-8
the name of the sample, as well as any observations made during the sampling or analysis. If
chlorine is not detected in the test, write not
detected.
A one-time demonstration of technician proficiency should be on file in the training records.
The one-time demonstration should include a
standard curve, a low-level measurement standard, and an annual performance evaluation
sample for chlorine and pH.
For turbidity sampling, all bottles must be thoroughly cleaned and rinsed with turbidity free
water prior to sample collection. Turbidity samples are collected typically during general tap
sampling, source water sampling from surface
water, and source water sampling from wells.
Refer to Sections 9.6.1, 9.6.4, and 9.6.5, respectively, for general sample collection procedures.
9.7.1.8. Preservation Requirements
There are no preservation requirements associated
with sampling pH, temperature, or chlorine residual. Ensure that samples for turbidity are cooled
to 6C.
9.7.1.9. Holding Time
Samples for pH, temperature, and chlorine residual must be analyzed immediately, which generally means within 15 minutes of sample collection. Samples for turbidity should be analyzed as
soon as possible after collection. If storage is
required, samples maintained at 6C can be
held for up to 48 hours.
9.7.2. Microbiological
This section covers specific sampling requirements for the following microbiologicals:
Coliforms
Cryptosporidium
Giardia.
9.7.2.1. Coliforms
Coliforms are a group of closely related bacteria
that are generally harmless, but do contain some
species that are human pathogens. They are
natural and common inhabitants of the soil and
ambient waters, such as lakes and rivers. Coliforms can be inactivated by treatment or die off
Page 9-10
Minimum Routine
Samples/Month*
25 1,000
1,001 2,500
2,501 3,300
Compliance with the TCR is based on the presence or absence of total coliform bacteria. If all
routine samples test negative (absent) for the
presence of total coliforms, no additional testing
is required for that monitoring period, regardless
of whether sampling is routinely conducted
monthly, quarterly, or annually. However, the
rule requires that total coliform-positive samples
(presence) be further tested for fecal coliform or
E. coli and that a set of three repeat samples be
collected for each total coliform-positive sample
monthly, quarterly, and annually. Systems that
collect one routine sample or fewer per month
must collect a fourth repeat sample. If total
coliforms are detected in any routine or repeat
sample, the sampler must collect at least five
routine samples the next month. Table 9-3 provides an abbreviated list of the required frequency
for repeat sampling.
Page 9-11
# of Repeat
Samples
# of Routine
Samples
Following
Month
1/month*
5/month
2/month
5/month
3/month
5/month
* Or fewer.
Page 9-12
with ice packs and deliver them directly. Samples analyzed by an off-site laboratory should be
shipped on ice via overnight service on the day
they were collected.
9.7.2.12. Cryptosporidium and Giardia
Cryptosporidium is a genus of protozoan parasites potentially found in water and other media.
The recent taxonomy of the genus Cryptosporidium includes two species that use humans as
hosts: C. hominis and C. parvum.
Giardia is a genus of protozoan parasites potentially found in water and other media. The recent
taxonomy of the genus Giardia includes one
species that uses humans as hosts: G. lamblia
(also called G. intestinalis or G. duodenalis).
Applicable Regulations. Under the 1996 SDWA
Amendments, EPA must supplement the existing
1989 SWTR with additional pathogen control
requirements. Several additions to the rule have
resulted in the Long-Term 2 Enhanced SWTR,
which focuses on the control of Cryptosporidium
and microbial pathogens.
MCLG. The Interim Enhanced Surface Water
Treatment Rule (IESWTR) has an MCLG of zero
or a 99% removal for systems that filter.
Number and Frequency of Drinking Water
Samples. Monitoring of source water is required
to determine the level of treatment for Cryptosporidium. Monthly samples are required for the first
2 years, with the level of Cryptosporidium determining the level of any subsequent treatment.
Most systems will not require additional treatment. A 6-year follow-up sample is required to
ensure continued compliance. Small systems can
monitor for E. coli and will monitor for Cryptosporidium only if the E. coli concentrations exceed
a specified level.
Sampling Locations. Samples are collected
from source water for distribution systems.
Analytical Methods. EPA Method 1623 can be
used to measure both Cryptosporidium and Giardia. Prior to analysis, the water sample must be
filtered and the extraneous materials retained on
the filter. Qualitative analysis is performed by
scanning each slide well for objects that meet the
Chapter 9 Drinking Water Sampling
cedure should be considered for bulk water samples that will be shipped off site because it minimizes the potential for water samples collected
during the summer to melt the ice in which they
are packed and arrive at the laboratory at > 20C.
If samples are shipped after collection at > 20C
with no chilling, the sample will not maintain the
temperature necessary to retard microbiological
activity and will not present a representative
sample for analysis.
PWSs shipping samples to off-site laboratories
for analysis should include in the shipping container a means for monitoring the temperature of
the sample during shipping to verify that the
sample did not freeze or exceed 20C. PakSense
labels adhere to the samples and provide accurate
readings of the temperature environment experienced by the samples in shipment.
Holding Time. Sample preparation must be
initiated within 96 hours of sample collection (if
shipped to the laboratory as a bulk sample) or
filtration (if filtered in the field). The laboratory
must complete elution, concentration, and purification in one workday. It is critical that these
steps be completed in one workday to minimize
the time that any target organisms present in the
sample sit in eluate or concentrated matrix. This
process ends with the application of the purified
sample on the slide for drying.
9.7.3.
Metals
EPA has determined that metals are health concerns at certain levels of exposure. Young children and pregnant woman are especially at risk
from high levels in their blood. Some of the most
pronounced effects in children are interference
with growth, deficits in IQ, and altered physical
and mental development.
Applicable Regulations. The SDWA has established MCLs for various metals (see Table 9-4).
The LCR applies to lead and copper and addresses the effects of plumbing materials on the
distribution system as well as ways to minimize
their concentration.
Table 9-4. Metal MCL or AL
Chapter 9 Drinking Water Sampling
Metal
Antimony
MCL (mg/L)
0.006
Arsenic
0.010
Barium
Beryllium
0.004
Cadmium
0.005
Chromium
0.100
Copper
AL= 1.3
Lead
AL= 0.015
Mercury
0.002
Selenium
0.05
Sodium
Thallium
20
0.002
emission spectra by optical spectrometry. Samples are nebulized, and the resulting aerosol is
transported to the plasma torch. Element-specific
emission spectra are produced by a radiofrequency inductively coupled plasma. The
spectra are dispersed by a grating spectrometer,
and the intensities of the line spectra are monitored at specific wavelengths by a photosensitive
device. Photocurrents from the photosensitive
device are processed and recorded by a computer
system.
System Size
(Population
Served)
Number of
Number of
Sites (Standard Sites (Reduced
Monitoring)
Monitoring)
3301 10,000
40
20
501 3,300
20
10
101
500
10
up to 100
Page 9-15
MCL (mg/L)
0.010
Chlorite
1.0
HAA5
0.060
TTHMs
0.080
Page 9-18
Constituents
Chlorinated
Nonchlorinated
Halocarbons &
Aromatics
THMs
Page 9-19
MCL
15 picocuries per liter
(pCi/L)
5 pCi/L
Uranium
30 g/L
made approximately 0.01 M in diethylenetriaminepentaacetic acid (DTPA), and the pH is adjusted to between 2.5 and 3.0. The sample is
transferred to a separatory funnel and equilibrated
with 1.50 milliliters of an extractive scintillator
containing a dialkyl phosphoric acid extracting
agent. Under these conditions, only uranium is
quantitatively transferred to the organic phase
while the extraction of undesired ions is masked
by the presence of DTPA. Following phase
separation, 1.00 milliliters of the organic phase is
sparged with dry argon gas to remove oxygen, a
chemical quench agent, and counted on a highresolution alpha-liquid-scintillation spectrometer
and multichannel analyzer (MCA). Radium-226
can be measured using EPA Method 903, and
radium-228 can be measured using EPA Method
904.
Sample Volume. Sample volumes will vary
depending on the analytical requirement. Generally, 1 gallon is collected per sample. Sample
volumes being collected must be confirmed with
the laboratory performing the analysis.
Bottle Type. Containers suitable for radionuclide
sampling are either a one pre-cleaned 1-gallon
Nalgene plastic bottle, or two pre-cleaned 2-liter
plastic bottles per sample.
Sampling Procedures. Radionuclide samples
typically are collected during general tap sampling source water, sampling from surface water,
and source water sampling from wells. Refer to
Sections 9.6.1, 9.6.4 and 9.6.5, respectively, for
general sample collection procedures.
Preservation Requirement. Preservation for
radionuclides is based on the method, parameter,
and state requirements. Cesium-134 is preserved
with HCl to pH < 2. Tritium and iodine-131 are
not chemically preserved. All other regulated
radionuclide parameters are preserved with nitric
acid to pH < 2. If preservation is not performed
in the field, the preservative can be added upon
arrival at the laboratory. The preservative must
be added within 3 days of collection, and analysis
must not begin until 16 hours after acidification.
Preservatives must be checked for the absence of
the radionuclides being monitored.
Chapter 9 Drinking Water Sampling
Chlorine
- Chlorine test kit or DPD test kit
Microbiological
- 120 milliliters plastic or glass
containers (sterilized)
- Sodium thiosulfate a preservative
- 10-liter collapsible containers
Metals
- First Draw
1-liter bottle, plastic or glass
Nitric acid a preservative
Warning signs to notify potential users
not to turn on taps during testing
period
- Service Line Samples
Pitcher or bucket
Sampling tap
1-liter bottle, plastic or glass
Nitric acid a preservative
Synthetic Organic Chemicals
- Sulfuric acid (for nitrate nonchlorinated water only)
- Sodium thiosulfate a dechlorinating
agent
- HCl a preservative
- Mercuric chloride a preservative
- 1-liter amber glass bottles with
Teflon-lined lids
Note: Samples will be considered a hazardous material
once mercuric chloride is added.
DBPs
- 40-milliliter amber vials with Teflonfaced silicone septa
- Ascobic acid a dechlorinating agent
- HCl a preservative if sampling for
halocarbons or aromatics
- 1-quart wide-mouth bottle
Page 9-21
Radionuclides
- HCl a preservative if sampling for
Cesium-134
- Nitric acid a preservative for all
other radionuclides except for tritium
and iodine-131
- 1-gallon or two 1-liter plastic or glass
bottles, volume dependent upon
sample.
Page 9-22
10.2. Scope
USTs
PCBs
Containers and drums
Oil spills
Waste characterization
Surface sampling
Sewage sludge.
10.2.1. USTs
UST sampling provides information used to
determine compliance with regulations applicable
to USTs that contain petroleum products and
stored chemical substances. If locating the USTs
is an issue, then an electromagnetic wave device,
electrical resistivity meter, or ground-penetrating
radar can be used to estimate the location of
buried tanks.
The following references contain guidance on
UST sampling:
Page 10-1
Chemical incompatibility
Leaking or deteriorated
Bulging
Explosive or shock sensitive
Laboratory waste.
As a precautionary measure, all unknown drums
should be handled and sampled with a minimum
of Level B protection (per 29 CFR 1910.120) to
characterize the content of the drums. The drum
survey should also address unstacked and unorganized drums.
WARNING: Opening drums presents a major health and
safety hazard. Accidents may include detonation, explosion, fire, vapor generation, and physical injuries. Proper
precautionary measures must be taken while performing
drum sampling.
Ignitability
Corrosivity
Reactivity
Page 10-3
Toxicity.
10.2.5.2. Ignitability
Ignitable hazardous wastes include the following:
(http://www.epa.gov/superfund/policy/remedy/pd
fs/93-45303fs-s.pdf).
10.3. Hazard and Safety Precautions
See Chapter 2 of this handbook for a discussion
of health and safety elements applicable to most
sampling programs. The following hazards,
discussed below, are specific to waste sampling:
Container hazards
USTs and other confined spaces
Explosive hazards.
10.3.1. Container Hazards
Reseal open bungs and drill openings as soon as
possible with new bungs or plugs to avoid vapor
release. If an open drum cannot be resealed,
place it into an overpack drum.
Bulging drums are extremely hazardous. Whenever possible, do not move drums that may be
under internal pressure, as evidenced by bulging
or swelling.
Laboratory packs (categorizing small containers
of chemicals, solvents, industrial supplies, etc. in
metal drums for disposal) can be an ignition
source for fires at hazardous waste sites, as they
sometimes contain shock-sensitive materials.
Treat such containers as explosive materials, and
use extreme care when opening these packs.
Prior to opening laboratory packs, make sure all
non-essential personnel are moved to a safe place.
Whenever possible, use a grappler unit constructed for explosives containment for initial
handling or sampling of such laboratory packs.
Sampling personnel should maintain continuous
communication with the Site Safety Officer until
operations are complete.
WARNING: If drums or cylinders show signs of swelling
or bulging, do not move or sample them until the pressure
can be relieved safely. If possible, relieve any excess
pressure prior to opening the drum by using a remotely
controlled device, such as a pneumatic impact wrench or
hydraulic penetration device. If pressure must be relieved
manually, place explosion-resistant plastic barriers between
the worker and the drums or cylinders.
WARNING: Only trained and certified explosives personnel should handle, sample, or test explosives or suspected
explosive materials.
10.4. Preparation
If the nature of the hazardous waste is unknown
(e.g., at an abandoned disposal site), sampling
personnel should take additional precautions to
protect themselves from direct contact with waste
materials. To characterize waste materials for
RCRA or to verify the contents in drums, cylinders, tanks, or transformers, it is important that
representative samples be collected and analyzed.
10.4.1. Preparation for UST Sampling
Before starting UST sampling, follow the hazard
and safety precautions specified in Section 10.3.
Prior to UST sampling, field personnel should
ensure there is no leakage of product from the
UST or related piping. If it is necessary to enter
into a tank or vault for sampling, strict procedures
for confined space entry should be followed by
qualified and experienced personnel.
10.4.2. Preparation for PCB Sampling
The toxic nature and degree of hazards posed by
PCBs require a high level of caution to be taken
during sampling. Appropriate protective gear and
clothing should be worn by sampling and support
personnel during sampling events. Proper gloves
should be used during sampling. Spill prevention
and control should be planned in advance if
transformer sampling is to be performed. Plastic
pads and sorbent materials should be available.
10.4.3. Preparation for Drum Sampling
Prior to initiation of a sampling event, all drums
should be inventoried. All available information
concerning each drum should be recorded in the
FLB/FN, including the following:
Type of drum
Contents
Total capacity estimate
Markings
Labels
Color
Origin
Condition.
Page 10-6
Each drum should be marked with a unique identification number that corresponds to the sample
container for present and future reference. Enamel spray paint is suitable for this purpose.
Photographs of the numbered drum are useful for
documenting the condition of the drum and providing a permanent record.
Type of cylinder
Contents
Total capacity estimate
Markings
Labels
Color
Origin
Condition.
Each cylinder should be marked with a unique
identification number that corresponds to the
sample container for present and future reference.
Photographs of the numbered cylinders are useful
for documenting the condition of the cylinder and
providing a permanent record.
10.4.5. Preparation for Storage Tank,
Vacuum Truck, Process Vessel, and
Similar Large Container Sampling
Prior to initiation of a sampling event, all containers should be inventoried. The following
information concerning each container should be
recorded in the FLB/FN:
Type of container
Total capacity estimate
Actual capacity (if container is open)
Chapter 10 Waste Sampling
Markings
Labels
Color
Origin
Condition
Existence and condition of ladders and
catwalks.
Each container should be marked with a unique
identification number that corresponds to the
sample container for present and future reference.
Enamel spray paint is suitable for this purpose.
Photographs of the numbered vessels are useful
for documenting the condition of the containers
and providing a permanent record.
The procedure for opening a large containment
vessel will vary with different containers. Ideally, large tanks and pressure/vacuum containers
should be vented and opened for sampling by the
tank operator familiar with tank access processes.
Most large tanks and vacuum trucks have valves
near the bottom of the tank and hatches near the
top. It is preferable to collect samples from the
top of a tank for several reasons. First, the integrity of valves near the bottom of the tank cannot
be assured; the valve may be immobile, break, or
become jammed in the open position, resulting in
an uncontrolled release of the tank contents.
Second, the contents of a large vessel may become stratified, and collecting a sample from the
bottom will not permit the sampling of each
strata. The preferred method is to access the tank
from the top to obtain a cross-sectional sample of
its contents.
While opening and sampling larger containment
vessels, precautions should be taken to ensure
personal health and safety. Accessing storage
tanks requires a great deal of manual dexterity.
Such sampling usually requires climbing to the
top of the tank through a narrow vertical or spiral
stairway while wearing protective gear and carrying sampling equipment. At least two persons
should perform the sampling: one to open the
hatch and collect the samples and the other to
stand back (usually at the head of the stairway)
and observe, ready to assist or call for help.
Page 10-8
1. Premeasure the area to allow for easier calculation of final results. If premeasuring is not
feasible, measurements may be taken after the
area is wiped.
2. Wearing a new pair of surgical gloves, remove the gauze pad from its sterile wrapping
container and soak the gauze pad with the appropriate solvent.
Page 10-11
10.5.4. Transformers
The many peculiarities associated with transformers warrant that they be considered separately
from drums and tanks. Because transformers
often are located in secured, out-of-the-way
locations, access may be a problem. A poweroperated scissor lift or cherry picker may be
needed to access pole-mounted transformers. In
other cases, the transformer may be in an underground cell.
Special precautions should be taken due to the
toxic nature and hazards posed by PCBs, which
may be present in a transformer. Appropriate
protection should be worn by sampling and
support personnel. To aid in spill prevention
and control, make sure to use plastic sheeting
and absorbent pads
WARNING: Prior to sampling, transformers must be
certified as off line and de-energized by an electrician
or other authorized person. Internal pressure should be
relieved before opening the transformer.
2.
Type of container
Estimated total capacity of individual
container
Actual container capacity
Markings, labels, color, origin, condition, etc.
Photographs may also be taken to provide a
permanent record.
Depending on the container location and position, it may be necessary to upright and/or relocate containers prior to sampling. Containers
that can be moved should be positioned so that
the opening, or bung, is upright, if the integrity
of the container will allow. Containers should
not be stacked.
WARNING: Drums containing liquid waste can be under
pressure or vacuum. A bulging drum should not be
moved or sampled until the pressure can be relieved
safely.
Page 10-15
tion by turning the T-handle upright and resting one end tightly on the locking block.
7. Slowly withdraw the sample from the waste
container with one hand while wiping the
sampler tube with a disposable cloth or rag
with the other hand.
8. Carefully discharge the sample into a suitable
sample container by slowly pulling the lower
end of the T-handle away from the locking
block with the lower end of the sampler positioned in the sample container.
9. Cap the sample container with a Teflonlined cap, label the container, and complete
the COC record and the FLB/FN.
10. Unscrew the T-handle of the sampler, and
disengage the locking block. Clean the sampler on site, or store the contaminated parts of
the sampler in a plastic storage tube for subsequent cleaning. Store used rags in plastic
bags for subsequent disposal.
10.5.6. Waste Pile Sampling
The protocol discussed below outlines general
procedures for collecting samples from waste
piles and other waste materials, equipment necessary for sampling, and adequate representation of
the material. This section also discusses factors to
consider when formulating a sampling plan. Due
to the many variables associated with waste
material sampling, exact procedures cannot be
outlined for every sampling situation. These
variables include the following: shape and size of
piles; size, compactness, and structure of the
waste material; and make-up. To determine the
correct sampling methodology, the chemical and
physical properties of a sample, the purpose of
the sampling event, analysis procedures, and the
intended use for the analyzed data should all be
considered when planning the sampling event.
10.5.6.1. Considerations for the Sampling Plan
The physical and chemical make-up of the waste
pile and the purpose for sampling should be
considered when planning the sampling event.
Considerations for creating a waste pile sampling
plan are presented below.
Page 10-17
especially useful if the waste pile is homogeneous. Compositing requires that equal amounts of
material from each sample be combined, and
ground, sieved, and/or sufficiently mixed so that
an aliquot sample can be removed for laboratory
analysis. To improve the quality of the composite
sample, follow the compositing considerations
offered in ASTM D6051, Standard Guide for
Composite Sampling and Field Subsampling for
Environmental Waste Management Activities.
If the concentration of a regulated material exceeds regulated levels, the entire waste pile
should be managed as regulated waste, or additional sampling and analyses should be performed
to define regulated and non-regulated material.
To avoid having to resample, field sampling
personnel should collect enough volume to provide for a different compositing scheme or additional individual analyses. This precaution requires initial field samples to be retained until the
laboratory results on the composited sample
become available.
When a waste pile is believed to be heterogeneous, individual random sampling is the preferred
sampling technique.
10.5.7. Containerized Solids
Sampling containerized solid materials (e.g.,
sludge, granulars, and powders) is accomplished
generally with one of the following samplers:
Scoop or trowel
Waste pile sampler
Grain sampler.
Each sample should be taken discretely. Depending on the objective of the sampling event (e.g.,
characterization for disposal), compositing samples in the field or laboratory on a weight/weight
basis prior to analysis may be permissible. The
procedure to collect samples using a waste pile
sampler is discussed in the previous section.
Use the following procedure to collect samples
using a scoop or trowel:
1. Open the container to be sampled.
Page 10-18
2. At specified intervals, take small, equal portions of sample from the surface and immediately below the surface.
3. Transfer the sample into a laboratory-cleaned
sample container, label the container, and
complete the COC record and the FLB/FN.
4. Clean the sampler on site, or store the contaminated sampler in a plastic storage tube for
subsequent cleaning. Store used rags in plastic bags for subsequent disposal.
A grain sampler consists of two slotted telescoping tubes, usually made of brass, stainless steel,
or high-density polyethylene. The outer tube has
a conical, pointed tip on one end that permits the
sampler to penetrate the material being sampled.
The sampler is opened and closed by rotating the
inner tube. Grain samplers are generally 61 100
centimeters long by 1.27 2.54 centimeters in
diameter. The following procedure is used to
collect samples using a grain sampler:
1. Open the container to be sampled.
2. While the sampler is in the closed position,
insert it into granular or powdered material or
waste being sampled from a point near a top
edge or corner, through the center, and to a
point diagonally opposite the point of entry.
3. Rotate the inner tube of the sampler into the
open position.
4. Wiggle the sampler a few times to allow
materials to enter the open slots.
5. Place the sampler in the closed position and
withdraw from the material being sampled.
6. Place the sampler in a horizontal position with
the slots facing upward.
7. Rotate and slide out the outer tube from the
inner tube.
8. Transfer the sample into a laboratory-cleaned
sample container, label the container, and
complete the COC record and the FLB/FN.
9. Clean the sampler on site, or store the contaminated sampler in a plastic storage tube for
subsequent cleaning. Store used rags in plastic bags for subsequent disposal.
Chapter 10 Waste Sampling
Page 10-20
10.6. QA/QC
See Chapter 3 of this handbook for information
on establishing an appropriate QA/QC protocol.
A QA/QC plan involves the establishment of a
sampling protocol, which is designed to minimize
sources of error in each stage of the process, from
sample collection to analysis and reporting of
analytical data. See Chapter 2 for information on
creating a SAP. Key elements of a SAP for waste
sampling are as follows:
Page 10-22
Page 11-2
Figure 11-1 Particle Size Ranges for Aerosols, Dusts, and Fumes
Source: Faith, W. L. and Atkinson, A. A., Jr
Page 11-3
Page 11-4
Page 11-5
Guidance Study Series, Vols. 1 4 are recommended for details on the various sampling methods. Sampling and Analysis of Airborne Pollutants, edited by Eric D. Winegar and Lawrence H.
Keith, also provides guidance in this area.
11.7.1. Direct Assessment
Generally, it is preferable to measure emission
rates directly rather than determine downwind
mass/volume concentrations, the reason being
that the data has more versatility for use in various modeling applications, where changes in
parameters such as meteorological conditions can
be evaluated. Direct measurements are also more
useful for determining long-term effects, determining National Priority List (NPL) status for
pollutants, and meeting permitting requirements.
They are most useful for volatile contaminants.
The preferred EPA method for these measurements is to set up an isolation flux chamber or
enclosure over a small surface area of the emission site. This method is recommended for:
Land surfaces
Non-aerated, non-mixed liquid surfaces
Aerated, mixed liquid surfaces
Fugitive emissions from processes including
leaks in seams, valves, ports, and controllers.
Advantages include:
Cost effective
Simple equipment requirements
Direct measurements
No models or estimates required
Generally better quality data
No upwind contamination and fewer meteorological interferences.
Disadvantages include:
Not always possible
Primarily used for volatiles materials
Must exercise caution in data extrapolation.
11.7.2. Indirect Assessment
The indirect assessment approach uses a variety
of samples from different ambient locations
relatively close to the source to estimate concentrations via dispersion modeling equations. There
are many models available, some developed for
stack emissions, and others for area sources. The
type of model determines the placement of samPage 11-6
Page 11-9
Page 11-13
The reagent can be in solution in a liquid impinger or "bubbler" or can be adsorbed on the surface of a porous solid. Liquid impingers require
considerable glassware that must be specially
cleaned, and the liquids must be handled in the
field under difficult conditions. In addition, the
impinger may have to be immersed in a bath of
ice water to prevent the evaporation of the reagent-containing liquid.
Cartridges of solid sorbents coated with derivitizing reagent can provide much higher collection
efficiencies than a liquid impinger. A variety of
sorbent media can be used including: silica gel,
glass beads, glass fiber filters, Amberlite XAD-2
resin, Florisil, Chromosorb P, Carbopak B,
and C18 coated silica. Although the solid phase
method is much superior to the impinger method,
the sampling is not without problems such as:
incomplete collection
reactivity of carbonyls
surface adsorption of carbonyls
artifact and interfering compound formation
blank contamination
variable rates of formation of derivatives for
various compounds
interference of ozone and sulfur dioxide
11.9.2.5. Nebulization/Reflux Concentration
This method is a modification of the bubbler/impinger methodology. In this case, instead
of bubbling air sample through a liquid scrubbing
solution, the liquid is nebulized to a fine mist
inside a glass bulb. Air is introduced through a
small orifice located in close proximity to the
nebulization tip and analytes of interest in the air
flowing through the mist are transferred to the
mist droplets. In the fine mist state, the surface
area for analyte contact is greatly increased,
resulting in significantly improved collection
efficiencies. A non-wettable filter (usually Teflon) collects and coalesces the mist back into the
bulb while passing scrubbed air out. The liquid
scrubber solution can either dissolve the analytes
of interest or chemically derivatize them.
Table 11-1 lists the EPA standard methods for
sampling ambient air and their respective collection media.
Page 11-15
Table 11-1 EPA Standard Air Contaminant Sampling Methods for Toxic Organic
Compounds
Method
Description
TO-1
TO-2
TO-3
TO-4
TO-5
TO-6
TO-7
TO-8
TO-9
TO-10
TO-11
TO-12
TO-13
TO-14
TO-15
Formaldehyde
Page 11-16
11.10. Particulates
Many toxic chemicals present in ambient air are
associated with solid particulates or aerosols.
Organic chemicals, such as semi-volatile organics and polar compounds, may adsorb to particulates or condense to varying degrees and exist
in a complex dynamic solid-vapor equilibrium
with particulate matter. Volatile metals, such as
cadmium and lead, in stack gases may condense
on the surface of particulates. Some toxic
compounds such as asbestos are present in
ambient air only as particulates. Air sampling
for particulates uses filtration, centrifugation, or
impaction to remove particles from the air (See
Figure 11-3 for an example of a typical particulate sampler). Certain adsorbed chemicals may
evaporate off the surface of the particles during
the capture process. Therefore, there is often
the need for a gas phase collection device (e.g.,
adsorbent) downstream from the particulate
capturing device. Analysis of both collection
media would be necessary to determine the total
amount of chemical present in the ambient air,
but the results may not describe the actual phase
distribution of the chemical in the air.
Page 11-17
Page 11-20
legally defensible form. When sampling begins, document the start time, flow rate, weather
conditions (ambient temperature, barometric
pressure, humidity, etc.), locations of sampling
equipment, and other pertinent information in
the Field Log Book/Field Notes. During sampling, check the weather conditions frequently
and enter them in the Log Book. Check the
sampling equipment periodically. Enter findings (e.g., sampler off, knocked over, etc.) in
the Log Book. If, at any time, the sampling
equipment must be moved, note the time of the
movement, the new locations, and the reasons
for movement. When sampling is completed,
record the time and ending flow rate. When
using a multiple part form, place part of the
form in the Log Book per the SAP or SOPs.
Include calculations (such as the volume of air
sampled, average flow rates, etc.) and pertinent
observations.
12. Ensure that all materials required for sampling are available in sufficient quantities for
the planned work.
Page 11-22
12.2. Scope
Sampling of water (and vapors) is commonly
conducted in groundwater treatment plants to
support decisions regarding compliance with
discharge permits and for making operational
decisions at the plant. Sampling may occur for
plant influent and effluent and intermediate
samples may be taken before and after specific
processes in the treatment train to:
Interstate Technology and Regulatory Cooperation (ITRC) Natural Attenuation of Chlorinated Solvents in Groundwater: Principles
and Practices (September 1999)
Technical Protocol for Evaluating Natural
Attenuation of Chlorinated Solvents in
Groundwater, EPA 600-R-98-128, 1998.
12.4.2. Enhanced Anaerobic Bioremediation
(EAB)
EAB usually involves injection of electron donor
formulations into groundwater in order to stimulate anaerobic conditions, and to promote reductive dechlorination of chlorinated solvents.
Electron donor formulations can include: corn
syrup, molasses, emulsified oils, whey, chitin,
etc. Introduction of electron donor results in
depletion of electron acceptors. Microorganisms
consume the most energetically favorable electron acceptors first (i.e., usually DO and nitrate),
followed by less favorable electron acceptors
such as sulfate. Chloroethenes, such as TCE,
become available as electron acceptors after the
more favorable electron acceptors have been
Chapter 12 Process Sampling
analysis. This testing is available thru commercially laboratories such as SiREM and Microbial
Insights.
For more information on qPCR testing see the
following reference:
used to supply DO to support aerobic biodegradation of hydrocarbons, such as benzene, toluene, ethylbenzene, and xylene (BTEX), in
groundwater. The chemicals usually contain
either magnesium- or calcium-peroxide based
formulations that, when hydrated, gradually
release DO into groundwater. Oxygen-release
chemicals can be applied in a number of different ways. In dry form, the chemicals can be
packed into socks that are suspended below the
water table, in wells. The dry powder can also
be spread across the surface at the bottom of
excavated areas for treatment of residual dissolved-phase hydrocarbon contamination; wetting of the area may be accomplished by applying water during backfilling. Alternatively, the
dry chemicals can be mixed with water to form a
slurry. The slurried material can then be delivered to groundwater via injection into existing
wells or by DPT. Injection of the slurry under
pressure usually results in distribution over a
greater area around the injection point (i.e.,
greater radius of influence) relative to passive
delivery techniques such as the suspended
sock method.
Hydrogen peroxide has also been used to supply
DO, and promote aerobic biodegradation of
organic contaminants. A solution of hydrogen
peroxide can be mixed into water that is being
injected, or the hydrogen peroxide solution can
be slowly metered into a well to provide a steady
supply of DO. The hydrogen peroxide will kill
microorganisms in the immediate vicinity of the
injection well, but it breaks down rapidly, and
releases oxygen as the main byproduct. The
concentration and flow rate of the hydrogen
peroxide solution must be carefully controlled to
limit inhibition of microbial activity to the immediate vicinity of the injection points.
The analytical requirements would include the
monitoring of DO and oxidation-reduction potential in groundwater as an indication of the
extent of chemical distribution. Such measurements are best made downhole using suitable
probes or low-flow sampling techniques. Monitoring of target contaminants in standard
groundwater samples would be an integral part
of the sampling and analysis program.
Page 12-4
and the soil samples are usually sent to an offsite laboratory. Incremental sampling of the soil
as it is placed in the container or stockpile will
yield more representative concentrations.
12.5.2. Landfarming
Landfarming (sometimes referred to as land
treatment) typically involves placement of contaminated soil onto a lined cell where it is periodically irrigated and tilled to promote biodegradation of organic contaminants. Landfarming
is a relatively slow treatment process that requires periodic monitoring to assess the progress
of treatment. The length of the treatment period
depends on what types of contaminants are
present, concentrations of contaminants, and on
the local climate. Treatment periods can range
from a few months to two or more years. In cold
climates, treatment operations are usually suspended during the winter and not resumed until
spring. The contaminants of concern represent
the primary monitoring parameters. In some
instances, it may be possible to correlate contaminant levels to a surrogate parameter such as
total petroleum hydrocarbons (TPH). There are
commercially available field analysis kits for
parameters such as TPH, and PAHs. The field
analysis kits can often be used to monitor the
progress of treatment, and to determine when to
collect confirmatory soil samples for laboratory
analysis. Other important monitoring parameters
include: soil moisture content, soil pH, and soil
nutrient levels (e.g., nitrogen and phosphorous).
Sampling is typically performed using hand tools
(e.g., trowel), and the confirmatory soil samples
are usually sent to an off-site laboratory. For
more information, refer to the following:
UFGS 02 55 00 (02160), Solidification/Stabilization (S/S) of Contaminated Material (04-2006); and ETL 1110-1-158, Treatability Studies for Solidification/Stabilization
of Contaminated Material.
12.5.3. Solidification/Stabilization
Solidification/Stabilization (S/S) typically involves blending contaminated soil with portland
cement and/or other additives, in order to reduce
the leachability of metals. A pug-mill is often
used to bend the soil and the cement. S/S does
not entail contaminant destruction, but sampling
and analysis is required to demonstrate that the
leachability of contaminants has been adequately
The contaminants of concern represent the primary monitoring parameters. Soil samples are
usually collected at a designated point of the
conveyor system for feeding the soil into the
LTTD unit, and from the treated soil stockpile.
Sampling can usually be performed using hand
tools, and the soil samples are usually sent to an
off-site laboratory. For more information, please
refer to:
Page 12-6
The number of process samples taken for analysis during the initial field sampling events should
be kept to a minimum to save time and costs.
Parameters that can be used as estimates for
other parameters should be used. For example,
the humic content of the soil or the COD may be
required for the final design of a selected
process. However, TOC is often recommended
in the earlier stage of investigation instead of
these parameters, as it is fairly easy to obtain and
should provide an estimate of these parameters
for the initial data analysis. For metals, consider
having a laboratory to analyze for all the metals
(approximately 30), as it may not cost any more
than analyzing for a selected few. Analyzing for
some parameters in the field may provide immediate information as to additional samples to take
to eliminate the need for an additional trip to the
field. It is recommended that the following
water parameters be routinely analyzed during an
early field sampling event: temperature, pH,
conductivity, turbidity, DO, and oxidationreduction potentials. These parameters can
provide much information on the water and are
easily measured with probes or other simple field
instruments. It is also recommended that soil
samples be collected for sieve analysis during the
initial sampling event. Sieve analysis can provide a rough estimate of the following parameters: plasticity, field capacity, bulk density,
particle density, permeability, porosity, and soil
classification.
ASTM D 7294 lists physical and chemical
treatment processes design data needed to evaluate, select, and design treatment processes for
remediation at contaminated sites. It is recommended that these data are collected prior to
evaluating remedies for large return/savings by
investing very little time and money up front.
This additional information will allow the decision makers to screen out technologies that are
not applicable (e.g., SVE in tight soil) or cost
effective, determine more accurate cost estimates, and save time and money by not having to
re-mobilize to collect data during the design
phase.
The analytical costs and time of obtaining these
samples will be less than that for obtaining conChapter 12 Process Sampling
taminant samples, because screening-level quality data is often sufficient, many tests are simple
and can be performed in the field, and a minimal
number of samples are needed to provide the
design data required. Additionally, if off-site
process parameters are expected to be the same
as on-site parameters, samples can be taken from
uncontaminated areas of the site and do not need
to be handled as hazardous waste.
ASTM D 7294 identifies the most important
parameters for a particular media and technology. Use the tables in ASTM D 7294 as a guide
in conjunction with the Treatment Technology
Profiles in the Remediation Technologies
Screening Matrix and Reference Guide at
http://www.frtr.gov/matrix2/section1/toc.html to
quickly search and screen technologies that may
be evaluated for site remediation later. The
process data needed to further evaluate these
technologies can then be obtained from ASTM D
7294 and can then be easily collected in the field
at the same time as the contaminant data collection.
The laboratory methods listed in ASTM D 7294
are well defined and consist primarily of Standard Methods, SW-846, and EPA 600 methods.
The field methods are not as well defined, and
the table gives general information on field
methods and their time and cost. Manufacturers
literature, the Internet and other information
should be used to select the field kits that best
meet the analytical and cost needs for that site.
For further information, see:
12.8. References
Page 12-9
Page 12-10
Field screening procedures are typically qualitative or semi-quantitative in nature and are performed using special screening equipment or
techniques, such as probes or portable hand-held
instruments and meters. Some field screening is
performed using field testing methods, and
special kits that are designed for use in a field
environment. Field screening is used to provide
a quick determination of the presence, magnitude, or absence of an analyte of concern. Field
screening provides preliminary results with
minimized costs on a real-time or near-real-time
basis. Because the quality control and analytical
sophistication of field screening is not as controlled as it is for laboratory testing, a representative set of split or duplicate samples should be
submitted to a laboratory for comparison of the
results.
13.2. Scope
The scope of this chapter includes a discussion
of field screening and field testing, and gives
examples of SOPs for several analyses that are
required by various regulations to be performed
in the field. Other analyses that are not required
for regulatory compliance also may be performed in the field. Field testing procedures and
strategies should be specified in the project SAP.
13.3. Background
A sampling event is conducted to collect sample
material for analysis of specific parameters to
determine site conditions. Some of these parameters can influence the characteristics of the
contaminants that need to be investigated and,
therefore, must be accurately measured at the
time of the sampling event. Certain parameters
require analysis in the field because of the potential for sample deterioration during transport to a
laboratory. Some parameters must be analyzed
in the field because they can fluctuate rapidly
with time and sample conditions. Parameters
that may require measurement in the field include pH, temperature, residual chlorine, specific conductance, oxidizer/cyanide test, and DO.
Matrix
Water
Total
Residual
Chlorine
Water
pH
Water,
aqueous
wastes
Wastewater,
aqueous
wastes
Water
13.4. Training
Personnel who will be performing any field
testing must be trained in sample collection,
preparation, and field testing methods, and demonstrate proficiency in the SOP for the test to be
completed. Training and proficiency must be
documented in accordance with the SAP. Navy
personnel should also document their training
following the Uniform Standards for Sampling,
OPNAVINST 5090.1C, Environmental and
Natural Resources Program Manual, Chapter 29.
Oxidizer/
Cyanide
Temperature
PID
Water, soil,
waste
Test Event
CERCLA and
drinking water
assessment
Drinking water and
wastewater
assessment
Waste profiling and
wastewater
assessment
Waste profiling and
wastewater
assessment
All water sampling
events
Preliminary
screening for
unknown volatile
organic
contaminants
Page 13-1
QAPP
Test methods
Calibration procedures
Reference standards
Materials and material preparation
Sample storage
Sample handling
Sample traceability
QC samples
Control charts
Data quality criteria
Detection limits
Recordkeeping
Data reporting procedures
Environmental conditions
Facility conditions and control
Personnel qualifications
Disposal
Safety.
Page 13-2
Specific Conductance
(Field Testing)
Prep By:
Approved By:
Effective Date:
CAUTION
This Standard Operating Procedure has been prepared as an example for this handbook and may not be specifically applicable to all activities or organizations. Any mention of trade names or commercial products does not constitute endorsement or recommendation for use.
Page 13-3
2.1
This procedure is applicable to drinking, ground, surface, and saline waters; and domestic and industrial waste. This
procedure is for field testing where needed; however, some regulations do allow this test to be performed in the laboratory.
RCRA and CERCLA require analyses to be performed immediately upon sample collection. Drinking water programs allow a
28-day holding time until analysis. See these regulations for sample preservation requirements.
3.0
Summary of Method
3.1
The determination of specific conductance gives a measure of the ability of an aqueous solution to carry an electric
current, which is related to the ions present in the aqueous solution.
3.2
The specific conductance of a sample is measured using a self-contained conductivity meter (Wheatstone Bridge-type
or equivalent).
3.3
Whenever possible, samples are analyzed at 25C. If samples are analyzed at different temperatures, corrections must
be made and results reported at 25C.
4.0
Interferences
4.1
Platinum electrodes can degrade and cause erratic results. When this happens, as evidenced by erratic results or flaking
of the platinum black, the electrode should be replaced.
4.2
The specific conductance cell can become coated with oil and other materials. It is essential that the cell be thoroughly
rinsed and cleaned between samples.
5.0
Equipment List
5.1
Conductivity Bridge (self-contained, Wheatstone Bridge-type or equivalent. Range 11,000 S/cm) with Conductivity
Cell (cell constant of 1.0, YSI #3403 or equivalent). Current METCAL calibration is required. Annual verification of cell
constant is required.
5.2
5.3
Thermometer - calibrated and able to read 0.1 degrees. (At a minimum, mercury in glass thermometers and dial-type
thermometers shall be checked annually against a National Institute of Standards and Technology (NIST)-traceable thermometer.)
5.4
FLB/FN
5.5
5.6
6.0
6.1
Potassium chloride (KCL) solution; 0.01M: Dissolve 0.7456 gram of predried (2 hours at 105C) KCL (reagent grade)
in distilled water, and dilute to 1 liter at 25C. Conductivity of this solution is 1,413 S/cm at 25C. Laboratory personnel can
prepare this solution, or an equivalent NIST-traceable reference standard may be purchased.
6.2
Distilled water. If doing RCRA Method 9050, deionized distilled water is required with conductivity of less than 1
mho/cm.
Page 13-4
7.1
Refer to the MSDS for details on chemical hazards and personal protection.
7.2
Minimum PPE, (i.e., chemical safety goggles and appropriately selected protective gloves) should be worn. Other PPE
(e.g., safety shoes, hard hat, respirator) will be dictated by the specific hazards of the sampling site.
7.3
8.0
Preparation
8.1
8.2
8.3
Follow the directions of the manufacturer for the operation of the instrument.
9.0
9.1.1
9.1.2 Calibrate conductivity meter prior to use, using KCl solution (see paragraph 6.1) at 25C and the table below to check
the accuracy of the cell constant and conductivity bridge:
Conductivity 0.01M KCl
C
S/cm
21
1305
22
1332
23
1359
24
1386
25
1413
26
1441
27
1468
28
1496
9.1.3
Meter reading
Temperature
9.1.4 The number and concentration of the standards used for calibration should be based on the testing needs for the field
activity. A single point check standard in the range of the sample concentrations to be measured may be used for field screening.
Page 13-5
Procedure
10.1
Obtain sample according to the appropriate sampling SOP, and pour into sample container with a minimum of aeration.
10.2
Rinse cell with distilled water. Rinse probe with remaining sample water.
10.3
10.4
10.5
10.6
10.7
Determine the temperature of samples. If the temperature of the samples is not 25C, make temperature correction in
accordance with the following guidelines:
If temperature of the sample is below 25C, add 2% of the reading per degree.
The more the sample temperature of the measurement deviates from 25C, the greater the uncertainty in applying the temperature correction.
10.8
Sample ID
Sample temperature, C
10.9
Recheck calibration with the KCl solution (see paragraph 6.1), and enter into conductivity meter log book.
11.0
QA/QC
11.1
11.2
Conductivity cell constant must be determined annually per Reference 12.2, Section 7.1.
11.3
Temperature variations and corrections represent the largest source of potential error.
11.4
Analyze calibration standards (see paragraph 6.1) after approximately every 15 samples, per RCRA method #9050A
(paragraph 8.2).
11.5
Run one duplicate sample for every 10 samples, per RCRA method #9050A (paragraph 8.3).
12.0
References
12.1
EPAMethods for Chemical Analysis of Water and Wastes. EPA-600/4-79-020 Method 120.1 (Specific Conductance
mhos at 25C) Editorial Rev., 1982. Applicable to drinking water and wastewater.
12.2
Test Methods for Evaluating Solid Wastes. SW-846, Method 9050A Specific Conductance. Applicable.
Page 13-6
Figure 13-2. Sample SOP for Field Determination of Total Residual Chlorine
Field Determination of
Total Residual Chlorine
Prep By:
Approved By:
Effective Date:
CAUTION
This Standard Operating Procedure has been prepared as an example for this handbook and may not be specifically applicable to all activities or organizations. Any mention of trade names or commercial products does not constitute endorsement or recommendation for use.
Page 13-7
Title: Standard Operating Procedure for Field Determination of Total Residual Chlorine.
2.0
2.1
The HACH DR 100 Colorimeter is a portable battery-powered colorimeter designed for field testing. This instrument is utilized to measure the total residual chlorine content of samples. The DR100 conforms to the requirements of
reference 11.1 using a 2.5-cm sample cell and DPD pillow-packed reagents for total residual chlorine determination. Reference 11.2 details operation and maintenance for the DR100.
2.2
This procedure is used to determine the level of residual chlorine for drinking and wastewater samples. Residual
chlorine in drinking water must meet specified requirements. In wastewater analysis, residual chlorine can possibly interfere
with some test procedures.
3.0
Summary of Method
3.1
Chlorine (hypochlorite ion, hypochlorous acid) and chloramines stoichiometrically liberate iodine from potassium
iodide at pH 4 or less. The liberated iodine reacts with N,N-diethyl-p-phenylene diamine (DPH) to produce a red-colored
solution. The solution is spectrophotometrically compared to a series of standards. The results are read in mg/l Cl.
4.0
Interferences
4.1
Interferences from oxidized manganese and copper are corrected by the addition of the DPD reagents. The method
inhibits trace metal catalysts. High concentrations of monochloroamine (combined chlorine) will not interfere with the total
residual chlorine test.
4.2
5.0
Equipment
5.1
5.2
Clippers.
5.3
5.4
5.5
5.6
5.7
5.8
5.9
FLB/FN
6.0
6.1
6.2
Stock Potassium Permanganate Solution (1000 ppm EquivalentChlorine Standard Solution). Place 0.891 gram
KMNO4 in a 1-liter volumetric flask, and dilute to 1 liter. Consult Reference 11.1 for preparation. This solution must be
refrigerated and has a shelf life of 6 months. This reagent can be prepared by laboratory personnel or purchased from commercial sources.
6.3
Page 13-8
Nitric Acid, 0.1N. This reagent can be prepared by laboratory personnel or purchased from commercial sources.
6.6
7.0
7.1
Refer to the MSDS for details on chemical hazards and personal protection.
7.2
Minimum PPE is chemical safety glasses and appropriately selected gloves. Hazards associated with the sample or
sampling site may require additional PPE.
7.3
8.0
8.1
Standard Preparation
8.1.1 Pipet 10.0 mL of the primary stock standardization solution potassium permanganate (paragraph 6.2) into a 100-mL
volumetric flask. Fill volumetric flask to mark with reagent (ASTM Type I or II) water and mix. This is the secondary stock
solution (equivalent 100 ppm chlorine).
8.1.2 Pipet 1.5 mL of secondary stock solution (paragraph 8.1.1) into a 100-mL volumetric flask. Fill flask to volume with
reagent (ASTM Type I or II) water, and mix. This will produce an equivalent total chlorine standard with a concentration of
1.50 mg/L.
8.1.3 Pipet 1.0 mL of secondary stock solution (paragraph 8.1.1) into a 100-mL volumetric flask. Fill the flask to volume
with reagent (ASTM Type I or II) water, and mix. This will produce an equivalent total chlorine standard with a concentration of 1.00 mg/L.
8.1.4 Pipet 50.0 mL of the 1.00 mg/L standard (paragraph 8.1.3) into a 100-mL volumetric flask. Fill the flask to volume
with reagent (ASTM Type I or II) water, and mix. This will produce a total chlorine standard with a concentration of 0.50
mg/L.
8.1.5 Pipet 10.0 mL of the 1.00 mg/L chlorine standard (paragraph 8.1.3) into a 100-mL volumetric flask. Fill the flask to
volume with reagent (ASTM Type I or II) water, and mix. This will produce a total chlorine standard with a concentration of
0.10 mg/L.
8.2
8.2.1 Using the DR100 and the procedure in paragraph 8.3.3, STEPS (1) through (10), analyze a blank (0.00 mg/L ASTM
Type I or II water) and the 0.10, 0.50, 1.00, and 1.50 mg/L standards. (8.1.2, 8.1.3, 8.1.4, 8.1.5).
8.2.2 After reading each standard, place the cell contents used for each reading in a flask, and titrate with standardized
ferrous ammonium sulfate (FAS) titrant. Record these values as the true standard concentrations.
8.2.3 Plot a calibration curve of measured (meter) values versus true values. This chart shall be kept with the meter and
updated annually, or when quality control data indicates potential errors.
8.3
Daily Standardization
Note: Prior to beginning this procedure, ensure reagents are not beyond expiration date.
8.3.1 Once the meter has been checked to ensure that it is in acceptable working condition, it is ready for daily standardization. The DR100 Colorimeter does not require a warm-up period. Both the mechanical zero and low battery indicator
check should be made with the meter in the same general position that it will be in when the measurements are made. (See
paragraph 10.3.3).
8.3.2
The DR100 Colorimeter shall be standardized prior to use each day at a minimum of 3 points that bracket the
Page 13-9
Standardization Steps
STEP (1) Open the light shield, turn the right set knob fully clockwise, and place the 1-cm cell holder (without the 1-cm cell
in the holder) in the left set position of the sample well. Close the light shield.
STEP (2) Hold the ON button down while adjusting the left set knob to align the meter needle with the arrow at the extreme
left of the scale arc. Remove the cell holder.
STEP (3) Fill a clean 2.5-cm sample cell with reagent (ASTM Type I or II) water. Cap the cell and place it into the sample
well. Press down firmly to seat the sample cell, and close the cell holder.
STEP (4) Hold the ON button down while adjusting the right set knob for a reading of 0.00 mg/L. Open the light shield, and
remove the sample.
STEP (5) Remove the cap from the sample cell used in STEP (3) and add the contents of a DPD total chlorine powder
pillow to the sample cell. Cap and shake it for 20 seconds. Allow at least 3 minutes but not more than 6 minutes for proper
color development. (This is a prepared standard of 0.00 mg/L or blank.)
Note: It is not necessary for all of the powder reagent particles to dissolve to obtain an accurate reading. Shaking the cell
dissipates bubbles that may form on the cell wall and interfere with the test results.
STEP (6) Place the cell containing the prepared standard from STEP (5) into the sample well. Press down firmly to seat the
sample cell, and close the light shield.
STEP (7) Hold the ON button down until the meter stabilizes.
STEP (8) Read the total chlorine concentration in mg/L from the upper (0.002.00) mg/L) scale. If the meter reading is 0.05
mg/L or less, then the meter is within the acceptable range and is to be reported as 0.00 mg/L.
STEP (9) Record this as a meter reading in the FLB/FN under the blank total chlorine concentration standard.
STEP (10) Remove the sample cell from the sample well, and rinse the inside of the sample cell and cap with reagent
(ASTM Type I or II) water at least two times to remove any residue.
8.3.4 Repeat STEPS (3) through (10) using the 0.50 mg/L and the 1.00 mg/L standards (prepared in 8.1) in place of the
ASTM Type I or II water. Record each meter reading in the FLB/FN. Refer to the calibration table to determine the true
values associated with the meter readings, and record in the FLB/FN. Corrected values must be within the acceptable range
of +0.05 units of the known standard concentration.
8.3.5 If the corrected value is outside of the acceptable range of +0.05 mg/L from the known standard concentration, then
another standard solution shall be prepared and the standardization repeated. If the corrected value remains outside of this
range, then it shall be assumed that the meter is malfunctioning. The Lab Director should be contacted for further instructions.
9.0
Procedure
9.1
9.1.1 Samples shall be collected in a clean glass or plastic container and tested on site within 15 minutes. No preservation
is necessary for on-site testing
9.1.2 Samples should have a pH between 6 and 7 for this procedure to be used. If necessary, an appropriate amount of
acid (0.1 N Nitric Acid) or base (0.1 N Sodium Hydroxide) that does not contain ammonium or chloride ions can be used to
Page 13-10
Prior to daily use, standardize meter using standardization procedure (see paragraph 8.3).
9.2
Sample Analysis
9.2.1 Perform STEPS (3) through (10) of paragraph 8.3.3 for each set of samples and if the meter is physically relocated
or disturbed during analysis of a sample set (any movement may offset the prism and invalidate the analyses). Analyze each
sample following STEPS (1) through (10) of paragraph 8.3.3.
9.2.2 Once the meter value for each sample has been determined, that value shall be found in the calibration curve/table
accompanying each meter. This gives the true total chlorine concentration. Record this true concentration in FLB/FN or
appropriate data sheet.
9.2.3 If the sample temporarily turns yellow when adding the DPD Total Chlorine Reagent or reads above the highest scale
division, the chlorine concentration is too high for the meter calibration. Any readings above 2.00 mg/L should be reported as
>2.00 mg/L. Chlorine concentrations may be approximated by additional sampling, dilution, and further analysis. The sample
also may be retained to determine if an interference exists or for reanalysis using a different test method.
10.0
10.1 Ten percent of the samples shall be analyzed in duplicate (split samples). Ten percent of the samples shall have
duplicate samples taken and analyzed (field duplicates). Record data in the FLB/FN or appropriate Data Sheet. Follow
QAPP for reporting results.
10.2 A calibration curve is prepared at least annually. When any meter measurement is made, the value from the meter
should be read to the nearest 0.05 units up to a meter reading of 1.50 mg/L. All values between 1.5 and 2.0 mg/L should be
read to the nearest 0.1 unit on the meter scale. The meter value obtained in this procedure should then be found on the
accompanying calibration curve to determine the true total residual chlorine concentration.
10.3 The HACH DR100 Colorimeter should have routine maintenance performed before it is standardized or used for
field measurements. The following maintenance steps cover the internal components to ensure that the meter is functioning
properly.
10.3.1 The DR100 Colorimeter uses four AA size batteries. These batteries should be replaced at least annually. The
meter should be tagged to indicate the date of the last battery change. Do not use the instrument when the Low Battery
indicator is lit. An indicator light that remains lit after batteries have been replaced may indicate that the internal lamp is
burned out. In any event, if the light remains on after batteries have been changed, the meter is not functioning correctly and
should not be used. The Lab Director should be contacted immediately.
10.3.2 While the meter is in the OFF position and as level as possible, the meter needle should align with the arrow at the
far left of the meter scale. To reset the meter needle, use a screwdriver to adjust the mechanical zero screw in the center of
the meter.
10.3.3 Other important considerations in obtaining accurate data are the condition of the sample cell holder and the sample
cells. The exterior of the sample cell holder and sample cells should be cleaned with an absorbent tissue before placing them
into the meter. Both the sample cell holder and the sample cell should be kept as clean and free of scratches as possible.
After each test, the sample cells must be rinsed thoroughly with ASTM Type I or II water and dried. At no time should the
sample cell be left in the meter after completion of a test. As with any analog output meter, the meter should be directly in
front of the operator and as level as possible to eliminate errors when reading the meter scale.
11.0
References
11.1 Standard Methods for the Examination of Water and Wastewater, 21st Edition; Method 4500-C1.G, DPD Colorimetric Method.
Page 13-11
Page 13-12
Daily Standardization
Date:_______________
_____________________
__________________________
_____________________
__________________________
_____________________
__________________________
Sample Analysis
Sample Description
Meter
(mg/L)
Corrected
(mg/L)
Initials/Date/Time
_____________________
_________________
________________
_____________________
_____________________
_________________
________________
_____________________
_____________________
_________________
________________
_____________________
_____________________
_________________
________________
_____________________
_____________________
_________________
________________
_____________________
_____________________
_________________
________________
_____________________
_____________________
_________________
________________
_____________________
_____________________
_________________
________________
_____________________
Page 13-13
Prep By:
Approved By:
Effective Date:
CAUTION
This Standard Operating Procedure has been prepared as an example for this handbook and may not be specifically applicable to all activities or organizations. Any mention of trade names or commercial products does not constitute endorsement or recommendation for use.
Page 13-14
Figure 13-3. Sample SOP for Field pH Measurements Using pH Paper (continued)
1.0
2.0
2.1
The pH paper method is used as a pH-screening method for aqueous wastes or in cases where pH measurements
using a meter are not possible.
2.2
This method is not applicable to wastes that contain components that may mask or alter the pH paper color change.
2.3
pH paper is not considered to be as accurate in measuring pH as a pH meter. Measurements taken using paper can
be used to define waste as corrosive or non-corrosive (pH < 2 or > 12.5) only if the measured values differ from either
threshold limit by a full pH unit. If readings within the ranges of either pH 13 or pH 11.513.5 are obtained using pH
paper, then a pH meter should be used if possible to determine whether the waste is corrosive.
3.0
Summary of Method
3.1
3.2
A more accurate pH determination is made using narrow-range pH paper whose accuracy has been determined by
using a series of buffers or by comparison with a calibrated pH meter.
4.0
Interferences
4.1
Certain waste may inhibit or mask changes in the pH paper. This interference can be determined by adding small
amounts of acid or base to a small aliquot of the waste and observing whether the pH paper undergoes the appropriate
changes.
4.2
Identification of Interferences
CAUTION: Addition of acid or base to samples may result in violent reactions or the generation of toxic fumes. Extreme
caution must be exercised. Do not perform this test when cyanides (or other toxic fumes) may be present or generated.
Perform this test in the field only with appropriate protective equipment and adequate ventilation.
4.2.1
4.2.2
4.2.3
Add acid drop wise to the first sample until a pH change is observed by noting the color change.
4.2.4
Add base drop wise to the second sample until a pH change is observed by noting the color change.
4.2.5 The observation of the appropriate color change is a strong indication that no interferences have occurred. Record
the results in the FLB/FN.
5.0
Equipment
5.1
5.2
5.3
5.4
FLB/FN.
6.0
6.1
6.2
Page 13-15
Figure 13-3. Sample SOP for Field pH Measurements Using pH Paper (continued)
6.3
Certified pH buffers.
6.4
6.5
6.6
7.0
7.1
7.2
For known or suspected corrosives where pH meter readings are not possible, wear the following PPE:
7.2.1
7.2.2
7.2.3
7.3
For known or suspected corrosives, an eyewash station and emergency shower should be located close to the work
area, and a two-member crew is required.
7.4
For water matrices (e.g., groundwater, surface water), minimum PPE is safety glasses.
7.5
8.0
Preparation of Equipment
8.1
Verify each batch of pH paper versus certified pH buffers or a pH meter that has been calibrated with certified
buffers.
8.2
9.0
Procedure
9.1
9.1.1 For drum sampling, particularly drums with unknown contents, examine the drum for its general condition. Note
condition in the FLB/FN.
9.1.2
Look for rusting, leaking, bulging, improperly secured cover, and other abnormal conditions.
9.1.4
9.2
9.2.1
9.2.2
pH measurements may or may not be taken directly from the source, depending on conditions.
9.2.3
Test the sample with wide range pH paper to determine the approximate pH. Record the results in the FLB/FN.
9.2.4
9.2.5
Take two measurements using the narrow range pH paper. Record the results in the FLB/FN.
9.2.6
pH measurements can be used to define a waste as a corrosive or non-corrosive only if the measured values differ
Page 13-16
Figure 13-3. Sample SOP for Field pH Measurements Using pH Paper (continued)
from either threshold limit (pH 2 or 12.5) by a full pH unit.
9.2.7 If readings in the ranges of either pH 13 or pH 11.513.5 are obtained, then the pH should be determined using a
meter.
10.0
Quality Control
10.1
10.2 Each batch of pH paper must be verified versus certified pH buffers or a pH meter that has been calibrated with
certified pH buffers.
11.0
Reference
11.1
Page 13-17
Figure 13-4. Sample SOP for Field pH of Aqueous Samples by Electrometric Measurement
Prep By:
Approved By:
Effective Date:
CAUTION
This Standard Operating Procedure has been prepared as an example for this handbook and may not be specifically applicable to all activities or organizations. Any mention of trade names or commercial products does not constitute endorsement or recommendation for use.
Page 13-18
Figure 13-4. Sample SOP for Field pH of Aqueous Samples by Electrometric Measurement (continued)
1.0
Title: Standard Operating Procedure for Field pH of Aqueous Samples by Electronic Measurement.
2.0
2.1
This method provides an SOP for field pH measurements and is applicable to aqueous samples and multiphasic
waste where the aqueous phase constitutes at least 20% of the total volume of the waste. The pH reading of a sample is the
logarithm of the reciprocal of the hydrogen ion concentration (hydrogen ion activity) in moles per liter.
3.0
Summary of Method
3.1
The pH of the sample is determined electrometrically using either a glass electrode in combination with a reference
potential or a combination electrode. The measuring device is calibrated using a series of standard solutions of known pH.
4.0
Interference
4.1
The glass electrode, in general, is not subject to solution interferences from color, turbidity, colloidal matter, oxidants, reductants, or moderate salinity.
4.2
Coatings of oily material or particulate matter can impair electrode response. Remove oily or particulate film before
measuring pH.
4.3
Temperature affects both the electrode output and the sample itself. Therefore, instrument calibration and sample
analysis should be performed as near to 25C as possible.
5.0
Equipment
5.1
Orion Research pH Meter Model 230A (or equivalent) or an appropriate portable pH meter with automatic temperature compensation.
5.2
5.3
5.4
Clean wipes.
5.5
5.6
FLB/FN.
6.0
6.1
pH 4.0, 7.0, 10.0 (at 25C) buffer solutions (buffer solutions to bracket expected sample values).
6.2
6.3
6.4
7.0
7.1
Wear appropriate PPE (minimum of chemical safety glasses and appropriately selected gloves).
7.2
7.3
8.0
8.1
Fill the pH electrode with fill solution, and precondition electrodes per the manufacturer's specifications of reference
Page 13-19
Figure 13-4. Sample SOP for Field pH of Aqueous Samples by Electrometric Measurement (continued)
11.2.
8.2
Remove the pH electrode from the storage solution, and thoroughly rinse with ASTM Type I or II water. Blot dry
with a clean wipe.
8.3
Position the pH probe in a sample of ASTM Type I or II water, and ensure the porous junction of the probe is
completely immersed.
8.4
Press the power key until the pH mode indicator is displayed. When the electrode is stable, the READY prompt will
be displayed. The pH of the ASTM Type I or II water should be approximately six.
8.5
dry.
Remove electrode from ASTM Type I or II water sample, rinse electrode with ASTM Type I or II water, and blot
8.6
Place the electrode in pH 7 buffer, and press the cal key. CALIBRATION will be displayed above the main
readout, and P1 is displayed in the lower field.
8.7
Wait for a stable pH display, then press the up arrow or down arrow key and the first digit will start flashing.
Scroll until the correct value appears in the first digit. Press yes. The second digit will start flashing. Scroll until the
correct value appears, then press yes. Continue in this manner until all digits have been correctly entered.
8.8
The display will remain frozen for 2 seconds; then, P2 will be displayed in the lower field indicating the meter is
ready for the next buffer (4 or 10 buffer).
8.9
Rinse the electrode with ASTM Type I or II water, and place the electrode into the second buffer. Wait for a stable
pH display, then enter the correct value.
8.10 The electrode slope (in percent) is then displayed in the main field with SLP in the lower field. The meter automatically advances to MEASURE mode.
8.11 Record the slope in the FLB/FN. The slope shall be from 95% 105%. If the slope is less than 95% or more than
105%, then recalibrate the pH meter.
8.12 Rinse the probe with ASTM Type I or II water, and place the electrode into the low range pH buffer solution.
Record the pH buffer and temperature reading. If the pH is not within 0.05 units of the solution value, then recalibrate the
pH meter.
8.13 Rinse the electrode with ASTM Type I or II water, and place the electrode into the high range pH buffer solution.
Record the pH buffer and temperature reading. If the pH is not within 0.05 units of the solution, then recalibrate the pH
meter.
8.14
Record calibration date and pH meter identification number in the appropriate FLB/FN.
Procedure
9.1
9.2
Agitate (without aeration) the sample, and decant an aliquot sufficient for analysis into a clean sample bottle.
9.3
Remove the pH electrode from the storage solution, thoroughly rinse the electrode with ASTM Type I or II water,
and blot it dry with a soft tissue.
9.4
9.5
Press the power key. When the electrode is stable, the READY prompt will be displayed and the temperaturecorrected value for the sample will be displayed. Record the pH, sample identification, and sample time in the FLB/FN.
9.6
If elemental analytes are to be determined, then preserve the remainder of the sample by acidifying with nitric acid
Page 13-20
Figure 13-4. Sample SOP for Field pH of Aqueous Samples by Electrometric Measurement (continued)
to a pH of 2.
10.0
Quality Control
10.1
10.2
Buffers shall be NIST traceable and shall have a current shelf life.
10.3
10.4 Calibration of mercury thermometers shall be checked at least annually against a NIST traceable certified thermometer.
10.5
The calibration of dial-type thermometers shall be checked at least quarterly against a NIST traceable thermometer.
11.0
References
11.1
Standard Methods for the Examination of Water and Wastewater, 21st Edition: Method 4500-H, pH Value.
11.2
11.3
Page 13-21
Date of Standardization:
__________________
Time of standardization:
__________________
Analyst:
__________________
Instrument Model:
__________________
Instrument S/N:
__________________
__________________
__________________
Buffer Solution
Temperature
Meter Reading
pH Corrected
(to 25C)
7.0
______________
__________________
___________________
4.0
______________
__________________
___________________
10.0
______________
__________________
___________________
Slope _________
Page 13-22
Prep By:
Approved By:
Effective Date:
CAUTION
This Standard Operating Procedure has been prepared as an example for this handbook and may not be specifically applicable to all activities or organizations. Any mention of trade names or commercial products does not constitute endorsement or recommendation for use.
Page 13-23
Title: Standard Operating Procedure for Oxidizer Field Testing for Cyanide Samples.
2.0
2.1
This SOP covers the procedure needed to test for oxidizers in aqueous samples requiring cyanide analysis. Oxidizers
are best removed at time of collection as they destroy/decompose most cyanides, causing a false low result.
3.0
Summary of Method
3.1
A few drops of sample are placed on potassium iodide-Starch test paper (KI starch paper). A blue color indicates
the presence of oxidizing agents, which may destroy or decompose cyanides. The sample must then be treated with ascorbic
acid to neutralize any oxidizing agents.
4.0
Interferences
4.1
None.
5.0
Equipment
5.1
Disposable droppers.
5.2
Sample containers.
5.3
FLB/FN.
6.0
6.1
6.2
6.3
7.0
7.1
Minimum PPE shall be chemical safety goggles (cyanide solutions can be corrosive) and protective gloves. Other
PPE will be dictated by the specific hazards of the sampling site (e.g., safety shoes, hard hats).
7.2
On returning from sampling, personnel will wash exposed skin with soap and water.
7.3
8.0
8.1
Take a drop from the potassium dichromate solution (paragraph 6.2) and test the KI starch paper. The strip should
turn blue.
9.0
9.1
9.2
With a disposable dropper, put a drop of sample on a strip of KI starch paper. A blue color on the strip indicates that
the sample contains oxidizing agents (e.g., chlorine).
9.3
If a blue color is observed, add ascorbic acid, a few crystals at a time, until a drop of sample produces no color
change to the KI starch paper.
9.4
Add an additional 0.6 grams of ascorbic acid for each liter of sample.
9.5
Page 13-24
Quality Control
10.1
11.0
References
11.1
Page 13-25
Prep By:
Approved By:
Effective Date:
CAUTION
This Standard Operating Procedure has been prepared as an example for this handbook and may not be specifically applicable to all activities or organizations. Any mention of trade names or commercial products does not constitute endorsement or recommendation for use.
Page 13-26
2.0
2.1
This method is applicable to drinking, surface waters, domestic and industrial waste, and other various aqueous
matrices.
3.0
Summary of Method
3.1
Temperature measurements may be made with any good grade of mercury - filled or dial type centigrade thermometer or thermistor.
4.0
Interferences
4.1
Temperature measurements must be made in the field because temperature is subject to change if there is a time
delay in taking the reading.
4.2
Time must be allowed for temperature reading to reach equilibrium (no observed change for 30 seconds).
5.0
Equipment
5.1
5.2
5.3
5.4
Clean wipes.
5.5
Rubber gloves.
5.6
FLB/FN.
5.7
PPE.
5.8
Sample containers.
6.0
6.1
7.0
7.1
Wear appropriate PPE. As a minimum, safety glasses and protective gloves should be worn.
7.2
Respiratory protection is generally not required for routine samples. However, personnel performing this procedure
should be aware of any potential volatile hazards that may require a respirator.
8.0
Procedure
8.1
8.2
8.3
Observe the temperature reading when equilibrium has been achieved (no change for 30 seconds).
8.4
8.5
8.6
Rinse the thermometer with water from the rinse water bottle, catching rinse in the waste container.
Page 13-27
9.0
Quality Control
9.1
9.2
The calibration of mercury thermometers shall be checked at least annually against a NIST-traceable certified
thermometer.
9.3
The calibration of dial-type thermometers shall be checked at least quarterly against a NIST-traceable thermometer.
9.4
Do not use thermometers where the indicating fluid has become separated.
10.0
Reference
10.1
Standard Methods for Examination of Water and Wastewater, 21st Edition: Section 2550 B, Temperature.
Page 13-28
____________________________
____________________________
Analyst:
____________________________
Temperature Log
Date/Time
Sample
Location
Reading
F / C
Analyst
Initials
Remarks
Page 13-29
Prep By:
Approved By:
Effective Date:
CAUTION
This Standard Operating Procedure has been prepared as an example for this handbook and may not be specifically applicable to all activities or organizations. Any mention of trade names or commercial products does not constitute endorsement or recommendation for use.
Page 13-30
Title:
2.0
2.1
To calibrate and perform periodic maintenance on a PhotoVac PID Model No. XXXX.
2.2
Calibration is required at the start of each day, and after each time maintenance is performed on the instrument
during the day (replacement of bulb or filter, etc.).
3.0
Summary of Method
3.1
Calibration the measuring device is calibrated using a series of standard gases of known concentration.
3.2
Maintenance requires the disassembly, replacement of minor components, and the reassembly of the instrument.
Note: Recalibration must be performed after each maintenance operation.
4.0
Equipment
4.1
4.2
Spare battery.
4.3
Battery charge.r
4.4
Spare bulb.
4.5
4.6
4.7
4.8
4.9
FLB/FN.
5.0
5.1
Methanol.
5.2
Cylinder of pure air, or activated carbon filter to make pure air and a sampling pump to fill the sampling bag.
5.3
6.0
6.1
6.2
6.3
Methanol is flammable.
7.0
7.1
Carefully unpack the instrument and examine it for physical damage that could have occurred in transit.
7.2
The units battery should be charged for 16 hours before use, since the battery can lose its charge during storage.
7.3
Completely empty a flexible air sampling bag (Tedlar or equivalent) using a vacuum (or sampling) pump.
Page 13-31
8.1
Perform any maintenance operations prior to calibration since disassembly/reassembly requires recalibration.
8.2
Any deviations from the following procedures shall be per the manufacturers instructions and noted in the FLB/FN.
8.3
Turn the power switch on to activate the unit. The pump should activate, making a continuous low humming sound.
8.4
Check the display for a LOW BAT indication (which means the battery should be replaced and/or recharged).
8.5
Allow the unit to operate for at least 2 minutes to come to equilibrium before calibrating.
8.6
Fill the bag with clean air (either Zero Air from a cylinder or air that has been passed through a tube of fresh
activated charcoal).
8.7
Connect the sample bag to the sampling port of the TIP (inlet port of the instrument). Set the SPAN control to
maximum, and adjust the ZERO knob until the display reads 0. Record the ZERO setting in the FLB/FN. Remove the
sample bag.
8.8
Fill a sample bag with calibration gas. Record the cylinder manufacturer, lot number, and the label information on
the chemicals present in the standard and their concentration in the FLB/FN.
8.9
Attach the sample bag to the sampling port of the TIP (inlet port of the instrument) and adjust the SPAN control
so that the display reads the same as the concentration on the label of the cylinder. Record both the SPAN setting and the
display in the FLB/FN. Remove the sample bag.
9.0
9.1
Any deviations from the following procedures shall be per the manufacturers instructions and noted in the FLB/FN.
CAUTION: Certain maintenance procedures may be performed in the field, however, these require the instrument to be
recalibrated. Maintenance procedures should be performed only by personnel who have been properly trained.
9.2
The TIP is fitted with a 15-m cartridge-style filter designed to capture particles that might otherwise be drawn into
the detector.
9.2.1
Never use instrument without the filter as the detector can be damaged.
9.2.2 Extended periods of operation in a dusty environment require frequent inspection of the filter for clogging and/or
absorption of particles carrying volatile material.
9.2.3 When a filter is clogged, the sensitivity of the instrument decreases since the sample flow-through is decreased. On
the other hand, when absorption of the volatile material occurs, a high background reading should be observed and consequently the need for an extreme zero resetting would be required.
9.2.4 The TIP response should be tested with and without the filter and the filter should be replaced if the response varies
by more than 10%.
9.3
To access the filter, hold the filter housing firmly at the base with a 9/16-inch wrench and unscrew the 1/8-inch
Swagelok connection for the sample inlet at the top of the housing with another 9/16-inch wrench.
9.4
9.5
9.6
10.0
10.1
Any deviations from the following procedures shall be per the manufacturers instructions and noted in the FLB/FN.
Page 13-32
The UV lamp should be cleaned if there is a significant loss of sensitivity not due to an obstructed filter.
10.3
10.4
Refer to the manufacturer's instructions for disassembly and detailed cleaning procedures.
CAUTION: Do not touch the bulb with bare skin, as this can leave an oil film on the bulb, which may damage the equipment.
CAUTION: Under certain circumstances, water can be sucked into the detector. Provided that the water is relatively clean,
this may not cause irreparable damage. Usually, the only corrective action needed is to have factory maintenance performed
by disassembling and cleaning the unit as soon as possible after the occurrence. Delay will likely result in corrosion of
internal parts.
10.5
10.6
10.7
When reassembling the instrument, be careful not to cross-thread the connections or damage the O ring seals.
10.8
10.8.1 If sensitivity is not recovered by cleaning or the lamp will not start, it is likely that a new lamp is required.
10.9
11.0
Quality Control
11.1 Quality control is maintained by strict adherence to these procedures performed by personnel who are trained and
familiar with the equipment.
11.2
Page 13-33
Page 13-34
Accreditation/certification status
Successful performance in related proficiency
testing (PT) programs, where available
Ability to meet project-specific QA/QC
requirements
Capacity to handle the specified number of
samples within the required turnaround time
Cost.
Once selected, communication with the laboratory prior to, during, and after sampling is essential
to ensure that reported results will meet regulatory requirements and can be used as intended.
14.2. Scope
This chapter addresses the technical aspects of
requesting laboratory testing services and selecting laboratories. Specifically, it contains guidance for preparing requests for quote (RFQ) or
scopes of work (SOW). The RFQ or SOW must
contain sufficient information to permit the laboratory to understand the requirement, provide a
complete and responsive quote, and perform the
tests and report the results in accordance with
relevant requirements. In the case of projects for
which a SAP has been prepared, the laboratory
should be provided with a copy of the plan at the
time the proposal or quote is solicited. The SOW
and project planning documents should be included or referenced in the laboratorys contract.
14.3. Responsibilities
The regulated party (e.g., permit holder or effluent
generator) ultimately is responsible for obtaining
valid test data. This includes the development of
Chapter 14 Guidelines for Requesting Laboratory Testing
procedure used must be documented in the laboratorys SOP for that method.
The following paragraphs discuss the selection of
parameters and methods for some common types
of compliance monitoring.
Wastewater. Parameters controlled under the
NPDES provisions of the CWA are listed in the
NPDES permit application, Form 2C. Testing
requirements including frequency, sample location, sampling method, and QC requirements,
also are described in the permit.
The approved test methods for wastewater, along
with sample holding times and preservation, are
listed in 40 CFR Part 136. In March 2007, EPA
proposed a number of new and revised analytical
methods used under both the CWA and Drinking
Water regulations. The proposed changes, found
in the Federal Register, March 12, 2007 (Volume
72, Number 47), include the following:
Note: When selecting or modifying methods, more extensive discussion is available in the EPA guidance document,
Guidance on Evaluation, Resolution, and Documentation of
Analytical Problems Associated with Compliance Monitoring, EPA 821-B-93-001, June 1993.
Page 14-4
14.9. Reporting
Laboratory reports must include a narrative describing the samples received, analyses, quality
control exceedances, and any unusual observations
made during analysis. The use of subcontractors
must be identified in the primary laboratorys final
report. The minimum recommended contents of
laboratory reports for compliance sampling include the following:
In the absence of client specified reporting criteria, the reporting requirements outlined below
shall be used for hard-copy data reports from the
laboratory. They are divided into mandatory
requirements for all printed data reports, and
optional requirements. Optional reporting requirements are those that may be required by a
specific project, depending upon the needs of the
project. The following elements are required:
cover sheet, table of contents, case narrative,
analytical results, sample management records,
and QA/QC information. Information for thirdparty review may be required depending on
project-specific requirements or the method being
used. The requirements below do not dictate
what records the laboratory should maintain.
1. Cover Sheet. The cover sheet shall specify
the following information:
2. Table of Contents. Laboratory data packages should be organized in a format that allows for easy identification and retrieval of
information. An index or table of contents
shall be included for this purpose.
3. Case Narrative. A case narrative shall be
included in each report. The purpose of the
case narrative is to describe any abnormalities
and deviations that may affect the analytical
results. It is also used to summarize any issues in the data package that need to be highlighted for the data user to help them assess
the usability of the data. The case narrative
shall provide:
COC records
Shipping documents
Records generated by the laboratory which
detail the condition of the samples upon
receipt at the laboratory (e.g., sample
cooler receipt forms)
Telephone conversation records associated
with actions taken or quality issues
Description of the sampling procedures if
the laboratory collected the sample.
6. QA/QC Information. The minimum internal
QC data package must include the following:
MS recovery
Page 14-6
LCS recoveries1
Surrogate recoveries (organics)
Serial dilutions (SD) percent difference
(metals)
Post-digestion spikes (PDS) recovery
(metals)
Project action levels, DQOs, Measurement
Quality Objectives (MQOs), and
associated acceptance criteria
Supporting documentation (e.g., run logs,
sample preparation logs, standard
preparation logs).
Analysis Time
BOD
0.5 day
5 days
Solids
0.5 day
1 day
1 day
0.5 day
0.5 day
0.5 day
per method
0.5 day
per method
Volatiles
0.5 day
1 day
Semi-volatile
organics
2 days
1 day
Pesticides
1 day
1 day
TCLP-metals
2 days
0.5 day
per method
TCLP-ZHEvolatiles
1 day
1 day
TCLPsemivolatiles
2 day
1 day
Radionuclides
2 days
1 to 15 days
Parameter
Wet chemistry
Metals, dissolved
Metals, total acid
digestion
Page 14-8
Appendix A.
Recommended Sampler
Limitations
a) Plastic
b) Glass
c) Teflon
None
Peristaltic Pump
Pond sampler
a) Grain sampler
b) Sampling trier
Trowel or scoop
Waste piles
a) Soil auger
b) Veihmeyer sampler
c) Kemmerer sampler
Note 1: These are only recommendations. Consult the applicable regulations to confirm sampler selection recommendations.
Page A-1
Sample Source
Matrix
Sampling Strategy
Drum
Liquid or solid
Liquid or solid
Solid (powder or
granular)
Soil
Soil
Waste piles
Solid
Pond, lagoon
Liquid or sludge
Liquid
Solid
Note 1: These are only recommendations. Consult the applicable regulations to confirm strategy recommendations.
Note 2: Refer to EPA QA/G5S for guidance on designing statistically relevant sampling plans.
Page A-2
Note 3: Refer to the USGSs National Field Manual for the Collection of Water-Quality Data for additional guidance
on collecting surface water samples.
Note 4: Refer to the USGSs Guidelines for Collecting and Processing Samples of StreamBed Sediment for Analysis
of Trace Elements and Organic Contaminants for the National Water Quality Assessment Program for additional
guidance on collecting surface water samples.
Page A-3
Page A-4
Appendix B.
Page B-1
Table B-1. Requirements for Sample Containers, Preservation, and Holding Times
(See Note 1 below)
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Alkalinity
Drinking
Water
200-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
14 days
SM2320
Alkalinity
Wastewater
200-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
14 days
EPA 310;
SM2320
Ammonia as
Nitrogen
Stormwater,
Surface water,
Wastewater
1-L glass or
polyethylene
bottles
H2SO4 to pH
< 2;
cool to 6C.
Fill to neck of
bottle.
28 days
EPA 350;
SM4500-NH3
Asbestos
Drinking
Water
2x 1-L glass
or polyethylene bottles
Cool to 6C.
Leave ample
air space in
the bottle (at
least 2.5 cm).
48 hours
EPA 100
Biochemical
Oxygen Demand
(BOD5)
Stormwater,
Surface water,
Wastewater
1-L glass or
polyethylene
bottles
Cool to 6C.
Fill to neck of
bottle.
48 hours
SM5210
Bromide
Solid and
Liquid Waste
100-mL glass
or polyethylene bottles
None required.
Fill to neck of
bottle.
As soon as
possible
SW-846
Methods
6500, 9056,
9211
Bromide
Wastewater
100-mL glass
or polyethylene bottles
None required.
Fill to neck of
bottle.
28 days
EPA 300;
SM4110
BTEX
Soils and
Sludges
2x 40-mL
vials (Note 4)
Per preparative
method. See
SW-846
Methods 5035,
5021, 5031,
5032.
14 days
Speciated
results from
VOC analysis: SW-846
Method 8260,
8015, 8021
BTEX
Wastewater
2x 40-mL
vials (Note 4)
Cool to 6C.
If residual
chlorine is
present, add
0.008%
Na2S2O3.
Adjust pH to 2
with HCl.
14 days
Speciated
results from
VOC analysis
(Note 6):
EPA 602,
624, 1624
Carbonaceous
Biochemical
Oxygen Demand
(CBOD5)
Surface water,
Wastewater
1-L glass or
polyethylene
bottles
Cool to 6C.
Fill to neck of
bottle.
48 hours
SM5210
Chemical Oxygen
Demand (COD)
Stormwater,
Surface water,
100-mL glass
bottles
H2SO4 to pH
< 2;
Fill to neck of
bottle.
28 days
EPA 410;
SM5220
Page B-2
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Cool to 6C.
Wastewater
Chloride
Drinking
Water
100-mL glass
or polyethylene bottles
None required.
Fill to neck of
bottle.
28 days
EPA 300;
SM4110,
SM4500-Cl
Chloride
Wastewater
100-mL glass
or polyethylene bottles
None required.
Fill to neck of
bottle.
28 days
EPA 300;
SM4110;
SM4500-Cl
Chloride
Groundwater,
Other
aqueous
waste
100-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
28 days
SW-846
Methods
6500, 9056,
9212, 9250,
9251, 9253
Chlorinated Acids
Drinking
Water
2x 1-L amber
glass bottles
fitted with
screw caps
lined with
Teflon
If chlorine is
present, add
0.008%
Na2S2O3. Seal
bottle and
shake vigorously for 1
minute. Cool to
6C, away
from light.
Fill to neck of
bottle.
Extract
within 14
days; analyze within
28 days of
extraction
EPA 515
Chlorinated Acids
Wastewater
2x 1-L amber
glass bottles
fitted with
screw caps
lined with
TFEfluorocarbon
If chlorine is
present, add
0.008%
Na2S2O3.
Cool to 6C.
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
Drinking
Water
500-mL glass
or polyethylene bottles
NA; analyze
immediately.
None.
15 minutes
SM4500-Cl
Drinking
Water
500-mL glass
or polyethylene bottles
NA; analyze
immediately.
None.
15 minutes
EPA 330;
SM4500-Cl
Wastewater
500-mL glass
or polyethylene bottles
NA; analyze
immediately.
None.
15 minutes
SM4500-Cl-
Coliform, Fecal
Drinking
Water
120-mL
borosilicate
glass or
plastic bottles,
pre-sterilized
plastic bags
If residual
chlorine is
present, add
0.008%
Na2S2O3. Cool
to < 10C
Leave ample
air space in
the bottle (at
least 2.5 cm).
6 hours
SM9221,
9222
Page B-3
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Coliform, Fecal
Surface water
and Wastewater
120-mL glass
or plastic
bottles, presterilized
plastic bags
If residual
chlorine is
present, add
0.008%
Na2S2O3. Cool
to < 10C.
Leave ample
air space in
the bottle (at
least 2.5 cm).
6 hours
SM9221,
9222
Coliform, Total
Drinking
Water
120-mL glass
or plastic
bottles or presterilized
plastic bags
If residual
chlorine is
present, add
0.008%
Na2S2O3. Cool
to 10C.
Leave ample
air space in
the bottle (at
least 2.5 cm).
6 hours
SM9221,
9222, 9223
Coliform, Total
Surface water,
Storm water
120-mL glass
or plastic
bottles or presterilized
plastic bags
If residual
chlorine is
present, add
0.008%
Na2S2O3. Cool
to < 10C.
Leave ample
air space in
the bottle (at
least 2.5 cm).
6 hours
SM9221,
9222
Conductivity
(Specific
Drinking
Water
500-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
28 days
SM2510
Groundwater
100-mL
plastic and
glass containers
None required.
None.
Analyze
immediately
SW-846
Method 9050
Corrosivity
Solid and
Liquid Waste
None required.
Fill per
sampling
plan.
None listed
SW-846
Method 1110
Cyanide
Drinking
Water
1-L glass or
polyethylene
bottles
NaOH to
Fill to neck of
bottle.
14 days
EPA 335;
SM4500-CN
Conductance)
Conductivity
(Specific
Conductance)
Holding
Time
Method
(Note 3)
to 6C. If
residual
chlorine is
present, add
small amounts
of Na2S2O3
solution (0.02
g/L) until
oxidizers are
neutralized. If
other oxidizing
agents are
suspected, refer
to Method
9010C for
preservation.
Page B-4
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Cyanide
Groundwater,
Other
aqueous
waste
1-L glass or
polyethylene
bottles
50%NaOH to
pH >12. If
oxidizing agent
is present, add
0.06 g ascorbic
acid per L.
Cool to 6C.
Fill to neck of
bottle.
14 days
SW-846
Method 9010,
9012, 9213
Cyanide
Solid and
other nonaqueous
100 g in a
glass jar
Cool to 6C.
None.
14 days
SW-846
Method 9013
Cyanide
Storm water,
Wastewater
1-L glass or
polyethylene
bottles
50% NaOH to
pH >12. If an
oxidant is
present, add
appropriate
reducing agent
as applicable to
the method.
Cool to 6C.
If other oxidizing agents are
suspected, refer
to Method
9010C for
preservation.
Fill to neck of
bottle.
14 days
EPA 335;
SM4500-CN
(48 hours if
not treated
for reducing
agents)
Dioxins and
Furans (PCDDs,
PCDFs)
Groundwater
4 x 1-L amber
glass bottles
with Teflon-lined
lids
Cool to 6C.
Keep away
from light. If
chlorine is
present, add
0.008%
Na2S2O3. If
pH is greater
than 9, adjust
to pH 7-9 with
sulfuric acid.
Fill to neck of
bottle.
Extract
within 30
days; analyze within
45 days of
extraction
SW-846
Methods
8280, 8290
Dioxins and
Furans (PCDDs,
PCDFs)
Sediment,
Soils, and
Sludges
250-mL wide
mouth glass
containers
with Teflon
lined lids
Cool to 6C
and keep in the
dark.
Fill to neck of
bottle.
Extract
within 30
days; analyze within
45 days of
extraction
SW-846
Methods
8280, 8290
Page B-5
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Dioxins and
Furans (PCDDs,
PCDFs)
Wastewater
4 x 1-L amber
glass bottles
with Teflon
lined lids
Cool to 6C.
Keep away
from light. If
chlorine is
present, add
0.008%
Na2S2O3. If
pH is greater
than 9, adjust
to pH 7-9 with
H2SO4.
Fill to neck of
bottle.
1 year
EPA 1613B
DBPs (Bromate)
Drinking
Water
40-mL amber
glass vials
28 days
EPA 300,
317, 326
DBPs (Chlorite)
Drinking
Water
40-mL amber
glass vials
14 days
(must arrive
at the
laboratory
w/in 48
hours of
collection at
6C or less)
EPA 300,
317, 326
DBPs (HAA5)
Drinking
Water
120-mL
amber glass
vials with
TFE-lined
caps
Crystalline or
aqueous NH4Cl
to produce 100
mg/L in
sample. Store
at 4C in the
dark.
28 days
EPA 552;
SM6251
DBPs(Trihalometh
anes)
Drinking
Water
2x 60-mL
glass vials
with Teflon
faced silicone
septum
Cool to 6C.
28 days
EPA 551,
502, 524
Fill to neck of
bottle with
minimal
aeration.
15 minutes
SM4500-O
Groundwater,
Surface water
and Wastewater
300-mL glass
stoppered
BOD bottles
Samples must
contain either
100 mg/L
ammonium
chloride or
Na2S2O3 as a
dechlorinating
agent. Refer to
selected
method for
preservation
requirements.
None required.
Page B-6
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Fluoride
Drinking
Water
100-mL
polyethylene
None required.
Fill to neck of
bottle.
28 days
EPA 300,
SM4110,
SM4500-F
Fluoride
Wastewater
100-mL
polyethylene
None required.
Fill to neck of
bottle.
28 days
EPA 300,
SM4110,
SM4500-F
Fluoride
Groundwater,
Other
aqueous
waste
300-mL
polyethylene
Cool to 6C.
Fill to neck of
bottle.
28 days
SW-846
Method 6500,
9056, 9214
Hardness
Drinking
Water
100-mL glass
or polyethylene bottles
HNO3 or
H2SO4 to
pH < 2; Cool
to 6C.
Fill to neck of
bottle.
6 months
EPA 130
Hardness
Wastewater,
Surface water
100-mL glass
or polyethylene bottles
HNO3 or
H2SO4 to
pH < 2; Cool
to 6C.
Fill to neck of
bottle.
6 months
EPA 130;
SM2340
Herbicides
Sediment,
Soils, and
sludges, Other
non-Aqueous,
Solid Waste
(concentrated)
250-mL wide
mouth glass
container with
Teflonlined lid
Cool to 6C.
Fill to neck of
bottle.
Extract
within 14
days; analyze within
40 days of
extraction
SW-846
Methods
8151, 8321
Herbicides
Groundwater,
Other
aqueous
waste
4 x 1-L amber
glass bottles
with Teflon- lined
lids
Cool to 6C.
Keep away
from light. If
chlorine is
present, add
3mL 10%
Na2S2O3 per
gallon.
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
SW-846
Methods
8151, 8321
Herbicides, TCLP
extract (Note 7)
Solid Waste
Three 1-L
wide mouth
amber glass
bottles with
Teflon lined lids
Cool to 6C.
Keep away
from light. If
chlorine is
present, add
3mL 10%
Na2S2O3 per
gallon.
Fill to neck of
bottle.
14 days from
field collection to TCLP
extraction; 7
days from
TCLP to
preparative
extraction;
analyze
within 40
days of
preparative
extraction
SW-846
Methods
1311, 8151,
8321
Page B-7
Parameter
Matrix
Sample
Containers
(Note 2)
Solid and
Liquid Waste
250-mL
amber wide
mouth glass
jar or wide
mouth polyethylene bottle
None listed.
Review sampling plan for
non-aqueous
wastes.
Fill with no
headspace
when volatiles are
suspected.
Check sampling plan.
Not
Drinking
Water
1-L certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
EPA 200,
SM3113
1-L certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
Groundwater,
Other
aqueous
waste
SW-846
Methods
6010, 6020,
6200, 6800,
7000, 7010
Metals
Solid waste
250-mL glass
jar
None required.
Fill to neck of
bottle.
6 months
SW-846
Methods
6010, 6020,
6200, 6800,
7000, 7010
Wastewater
1-L certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
SM3111;
EPA 200;
SM3113,
SM3120
Metals, Calcium
Drinking
Water
1-L certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
EPA 200,
SM3500-Ca,
SM3111;
SM3120
Metals, Calcium
Wastewater
1-L certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
SM3111,
SM3120,
SM3500-Ca
Metals, Calcium
Groundwater,
Other
aqueous
waste
1-L certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
SW-846
Method 6010,
6020, 6200,
6800, 7000
Ignitability
Metals
(Lead and Copper)
Metals
Metals
(Lead and Copper)
Preservation
Filling
Instructions
Holding
Time
established
Method
(Note 3)
SW-846
Method 1010,
1020, 1030;
ASTM D-9379, D-93-80,
D3278-78
Page B-8
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Metals, Calcium
Solid waste
250-mL
certified
metal-free
glass or
polyethylene
bottles
None required.
Fill to neck of
bottle.
6 months
SW-846
Method 6010,
6020, 6200,
6800, 7000
Metals, Dissolved
Groundwater
1-L certified
metal-free
glass or
polyethylene
bottles
Filter through
0.45-m filter.
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
SW-846
Method 6010,
6020, 7000,
7010
Metals, Dissolved
Stormwater
and Wastewater
1-L certified
metal-free
glass or
polyethylene
bottles
Filter through
0.45-m filter.
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
EPA 200;
SM3113,
SM3120
Groundwater,
Other
aqueous
waste
500-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
24 hours
SW-846
Methods
6800, 7195,
7196, 7197,
7198, 7199
Soils and
Sludges
250-mL glass
jar
Cool to 6C.
Fill to neck of
bottle.
30 days
SW-846
Methods
6800, 7195,
7196, 7197,
7198, 7199
Wastewater
1-L certified
metal-free
glass or
polyethylene
bottles
NaOH to pH of
9.3-9.7;
Cool to 6C.
Fill to neck of
bottle.
28 days
EPA 218;
SM3111C,
SM3500-Cr
Metals, Mercury
Drinking
Water
250-mL
certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2. Unpreserved
samples may
be sent to the
laboratory
within 2
weeks, then
acid preserved
and held 16
hours before
analysis.
Fill to neck of
bottle.
28 days
EPA 245;
SM3112
Metals, Mercury
Groundwater,
Other
aqueous
waste
500-mL glass
or polyethylene bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
28 days
SW-846
Method 7470
Holding
Time
Method
(Note 3)
Page B-9
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Metals, Mercury
Sediment,
Solid, Semisolid waste
250-mL glass
jar
Cool to 6C
Fill to neck of
bottle.
28 days
SW-846
Methods
7470, 7471,
7474
Metals, Mercury
Wastewater
and Storm
water
500-mL
certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2. Unpreserved
samples may
be sent to the
laboratory
within 2
weeks, then
acid preserved
and held 16
hours before
analysis.
Fill to neck of
bottle.
28 days
EPA 245;
SM3112
(CVAA
methods)
Metals, Primary
(As, Sb, Ba, Be,
Cd, Cr, Ni, Tl, Se)
Drinking
Water
1-L certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2. Unpreserved
samples may
be sent to the
laboratory
within 2
weeks, then
acid preserved
and held 16
hours before
analysis.
Fill to neck of
bottle.
6 months
EPA 200
Metals, Secondary
(Al, Fe, Mn, Ag,
Zn)
Drinking
Water
1-L certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2. Unpreserved
samples may
be sent to the
laboratory
within 2
weeks, then
acid preserved
and held 16
hours before
analysis.
Fill to neck of
bottle.
6 months
EPA 200;
SM3120
Page B-10
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Metals, TCLP
extract (Note 7)
Solid Waste
Three 1-L
wide mouth
glass bottles
Cool to 6C.
HNO3 to pH <
2.
Fill to neck of
bottle.
Metals: 6
months from
field collection to TCLP
extraction; 6
months from
TCLP
extraction to
analysis:
Mercury: 28
days from
field collection to TCLP
extraction;
28 days to
analysis
SW-846
Method 1311,
6010, 6020
Metals, Total
Storm water,
Surface water,
and Wastewater
1-L certified
metal-free
glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
EPA 200;
SM3111;
SM3113;
SM3120
Metals, Total
Sediment,
Soils and
Sludges
250-mL wide
mouth glass
or polyethylene jar
None required.
Fill to neck of
bottle.
6 months
SW-846
Methods
6010, 6020
Metals, Total
Groundwater,
Other
aqueous
waste
1-L glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
SW-846
Methods
6010, 6020
Nitrate
Drinking
Water
100-mL glass
or polyethylene
Cool to 6C.
Fill to neck of
bottle.
48 hours
EPA 300;
SM4110,
SM4500NO3
Nitrate
Wastewater,
Surface water,
Storm water
100-mL glass
or polyethylene
Cool to 6C.
Fill to neck of
bottle.
48 hours
EPA 300;
EPA 352;
SM4110;
SM4500NO3
Nitrate
Groundwater,
Other
aqueous
waste
1-L Teflon,
plastic, glass
Cool to 6C.
Fill to neck of
bottle.
48 hours
SW-846
Method 6500,
9056, 9210
Nitrite
Drinking
Water
100-mL glass
or polyethylene
Cool to 6C.
Fill to neck of
bottle.
48 hours
EPA 300;
SM4110,
4500-NO2 ;
SM4500NO3
Page B-11
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Nitrite
Wastewater
100-mL glass
or polyethylene
Cool to 6C.
Fill to neck of
bottle.
48 hours
EPA 300;
SM4110,
SM4500NO2 ;
SM4500NO3
Nitrite
Groundwater,
Other
aqueous
waste
100-mL glass
or polyethylene
Cool to 6C.
Fill to neck of
bottle.
48 hours
SW-846
Method 9056,
9216
Nitroaromatics
and Nitrosamines
(Explosives)
Wastewater
1-L amber or
foil wrapped
glass bottles
with TFE
lined cap
Cool to 6C;
if residual
chlorine
present add
0.008%
Na2S2O3. Store
in dark
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
EPA 625,
SM6410
Nitroaromatics
and Nitrosamines
(Explosives)
Groundwater
4 x 1-L amber
glass bottles
with Teflon
lined screw
cap
Cool to 6C;
if residual
chlorine is
present, add
0.008%
Na2S2O3. Store
in dark.
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
SW-846
Methods
8270, 8330,
8091
Nitroaromatics
and Nitrosamines
(Explosives)
Concentrated
Waste Samples, Soils,
and Sediments
250-mL
amber wide
mouth glass
with Teflon-lined lid
Store in the
dark at 6C.
Fill to neck of
bottle.
Extract
within 14
days; analyze within
40 days of
extraction
SW-846
Methods
8270, 8330,
8091
Soils and
Sludges
250-mL wide
mouth glass
container
fitted with a
TFE-lined
screw cap
HCl to pH < 2
for samples
with aqueous
layers.
Cool to 6C.
Fill to neck of
bottle.
28 days
SW-846
Method 9071
Surface water,
Storm water,
Wastewater
1-L wide
mouth glass
container
fitted with a
Teflon-lined
cap
H2SO4 or HCl
to pH < 2. Cool
to 6C.
Fill to neck of
bottle.
28 days
SM5520,
EPA 1664
Orthophosphate
Drinking
Water
100-mL glass
or polyethylene bottles
H2SO4 to pH
< 2.
Cool to 6C.
Fill to neck of
bottle.
28 days
EPA Method
365
Page B-12
Parameter
Orthophosphate
Orthophosphate
PCBs
Matrix
Drinking
Water
Surface water,
Wastewater
Drinking
Water
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
100-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
Filter within
15 minutes.
EPA Method
300; SM4110;
SM4500-P
100-mL glass
or polyethylene bottles
Cool to 6C.
4 x 1-L amber
glass bottles
with Teflon-lined
lids
If chlorine is
present, first
add 50 mg/L of
sodium sulfite.
Adjust the
sample to pH <
2 by adding 6N
HCl. Cool
48 hours
Fill to neck of
bottle.
Filter within
15 minutes.
48 hours
EPA 365,
EPA 300;
SM4110;
SM4500-P
Fill to neck of
bottle.
Extract
within 1
year; analyze within 1
year of
extraction
to 6C.
PCBs
Groundwater,
Other
aqueous
waste
4 x 1-L amber
glass bottles
with Teflon-lined
lids
Cool to 6C.
Keep away
from light. If
chlorine is
present, add
3mL 10%
Na2S2O3 per
gallon.
Fill to neck of
bottle.
Extract
within 1
year; analyze within 1
year of
extraction
SW-846
Method 8082
PCBs
Sediment,
Soils and
Sludges, and
other nonaqueous
Cool to 6C.
Keep away
from light.
Fill to neck of
bottle.
Extract
within 1
year; analyze within 1
year of
extraction
SW-846
Method 8082
PCBs
Wipe Samples
Cool to 6C.
Not established
SW-846
Method 3500,
3540, 3550,
8082
PCBs
Wastewater
1-L amber
glass bottles
fitted with
Teflonlined screw
cap
Cool to 6C,
if residual
chlorine
present add
0.008%
Na2S2O3.
Fill to neck of
bottle.
Extract
within 1
year; analyze within 1
year of
extraction
EPA 608,
625, SM6410
Page B-13
Parameter
PCBs (screening)
Pesticides
(Organochloral)
Matrix
Drinking
Water
Drinking
Water
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
2 x 1-L amber
glass bottles
HgCl2 to 10
mg/L. If
chlorine is
present, add
0.008%
Na2S2O3. Seal
bottle and
shake vigorously for 1
minute. Cool to
6C.
Fill to neck of
bottle.
Extract
within
1year;
analyze
within 1
year0 days
of extraction
2x 1-L amber
glass bottles
Residual
chlorine in the
sample should
be reduced by
adding 50
mg/L of
sodium sulfite.
Adjust the
sample to pH <
2 by adding 6N
HCl. Cool
Fill to neck of
bottle.
Extract
within 14
days; analyze within
40 days of
extraction
Method
(Note 3)
EPA 508
EPA 508
to 6C.
Pesticides
Groundwater
Four 1-L
amber glass
bottles with
Teflonlined lids
Cool to 6C.
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
SW-846
Method 8081,
8085
Sediment,
Soils and
Sludges,
Other NonAqueous
250-mL wide
mouth glass
container with
Teflon-lined
lid
Cool to 6C.
Fill to neck of
bottle.
Extract
within 14
days; analyze within
40 days of
extraction
SW-846
Method 8081,
8085
Wastewater,
Surface water,
Storm water
1-L glass
bottles with
Teflon-lined
cap
NaOH or
H2SO4 to pH 59; Cool to
6C (Note 5).
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
SM6630;
EPA 608
(Organochloral)
Pesticides
(Organochloral)
Pesticides
(Organochloral)
Page B-14
Parameter
Pesticides
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Drinking
Water
1-L glass
containers
If residual
chlorine is
present, add
0.008%
Na2S2O3. Seal
bottle and
shake for 1
min.
Cool to 6C.
Keep away
from light.
Fill to neck of
bottle.
Extract
within 14
days; analyze within
14 days of
extraction
EPA 507
Groundwater
Four 1-L
amber glass
bottles with
Teflon-lined
lids
Cool to 6C.
Keep away
from light. If
chlorine is
present, add
3mL 10%
Na2S2O3 per
gallon.
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
SW-846
Method 8085,
8141
Pesticides, TCLP
extract (Note 7)
Solid Waste
Three 1-L
wide mouth
amber glass
bottles with
Teflon-lined
lids
Cool to 6C.
Keep away
from light. If
chlorine is
present, add
3mL 10%
Na2S2O3 per
gallon.
Fill to neck of
bottle.
14 days from
field collection to TCLP
extraction; 7
days from
TCLP to
preparative
extraction;
analyze
within 40
days of
preparative
extraction
SW-846
Method 1311,
8141, 8085
pH
Drinking
Water
None required.
None.
Analyze in
field
EPA 150,
+
SM4500-H
pH
Groundwater,
Other
aqueous
waste
50-mL glass
or polyethylene bottles
None required.
None.
Analyze
immediately
SW-846
Method
9040C, 9045
pH
Soils and
Sludges
250-mL
amber wide
mouth glass
jar or wide
mouth polyethylene
bottles
None required.
None.
Analyze
immediately
SW-846
Method 9040,
9045
pH
Storm water,
Surface water,
Wastewater
50-mL glass
or polyethylene bottles
None required.
None.
Analyze
within 15
minutes
EPA 150;
+
SM4500-H
(Organophosphorus)
Pesticides
(Organophosphorus)
Page B-15
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Phosphorus
Surface water,
Storm water
100-mL glass
or polyethylene bottles
H2SO4 to pH <
2.
Cool to 6C.
Fill to neck of
bottle.
28 days
EPA 365;
SM4500-P
Polynuclear
Aromatic
Groundwater
4 x 1-L amber
glass bottles
with Teflon-lined
lids
Cool to 6C.
Keep away
from light. If
chlorine is
present, add
3mL 10%
Na2S2O3 per
gallon.
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
SW-846
Method 8100,
8270, 8410
Wastewater
4 x 1-L glass
bottles, amber
with TFElined cap
If residual
chlorine is
present, add
0.008%
Na2S2O3.
Cool
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
EPA 610,
625, 1625;
SM6410,
6440
Hydrocarbons
(PAHs)
Polynuclear
Aromatic
Hydrocarbons
(PAHs)
Holding
Time
Method
(Note 3)
to 6C.
Radiological Tests
(alpha, beta,
radium)
Groundwater
1-L glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
SW-846
Methods
9310, 9315,
9320
Radiological Tests
(alpha, beta,
radium)
Drinking
Water
1-L glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
EPA 900
(gross alpha,
beta); EPA
903 (radium226), EPA
904 (radium228)
Radiological Tests
(alpha, beta,
radium)
Drinking
Water
1-L glass or
polyethylene
bottles
HNO3 to pH <
2.
Fill to neck of
bottle.
6 months
SM7110
(alpha, beta),
C (gross
alpha);
SM7500-Ra
B, C (radium226), D
(radium-228)
Reactivity
Solid Waste
Two 250-mL
amber wide
mouth glass
jars or wide
mouth polyethylene
bottles
50% NaOH to
pH >12. Store
at 6C.
Fill with no
headspace
and per
sampling
plan.
Analyze as
soon as
possible
SW-846
Method 9010,
9012, 9013,
9014 for
cyanide
Page B-16
Parameter
Sample
Containers
(Note 2)
Preservation
Solid Waste
Two 250-mL
amber wide
mouth glass
jars or wide
mouth polyethylene
bottles
Fill with no
headspace
and per
sampling
plan.
Analyze as
soon as
possible
SW-846
Method 9030,
9031, 9215
for sulfides
Salinity
Surface water
None required.
None.
Analyze in
field
EPA 430/986-004
Semivolatile
Organics
Drinking
Water
Two 1-L
amber glass
bottles
Residual
chlorine should
be reduced at
the sampling
site by addition
of 40-50 mg of
sodium sulfite.
The sample pH
is adjusted to <
2 with 6N HCl.
Cool to 6C.
Fill to neck of
bottle.
Extract
within 14
days; analyze within
30 days of
extraction
EPA 525
Semivolatile
Organics
Groundwater,
Other
aqueous
waste
Four 1-L
amber glass
bottles sealed
vials
equipped with
unpierced
Teflon-lined
septa
Cool to 6C.
Keep away
from light. If
chlorine is
present, add
3mL 10%
Na2S2O3 per
gallon.
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
SW-846
Method 8270
Semivolatile
Organics
Soils and
Sludges,
Sediment, and
Other NonAqueous
250-mL wide
mouth glass
container with
Teflon lid
Cool to 6C.
Fill to neck of
bottle.
Extract
within 14
days; analyze within
40 days of
extraction
SW-846
Method 8270
Semivolatile
Organics
Storm water
1-L amber
glass bottles
with Teflon-lined
caps
If chlorine is
present, first
add 0.008%
Na2S2O3. Cool
to 6C and
keep in the
dark.
Fill to neck of
bottle.
Extract
within 7
days; analyze within
40 days of
extraction
EPA 625,
1625;
SM6410
Semivolatile
Organics
Concentrated
Waste Samples
125-mL wide
mouth glass
container with
Teflon lid
None required.
Fill to neck of
bottle.
Extract
within 14
days; analyze within
40 days of
extraction
SW-846
Method 8270
Reactivity
Matrix
(releasable sulfide)
(Note 6)
Filling
Instructions
Holding
Time
Method
(Note 3)
Page B-17
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Semivolatile
Organics, TCLP
extract (Note 7)
Solid Waste
Three 1-L
wide mouth
amber glass
bottles with
Teflon-lined
lids
Cool to 6C.
Keep away
from light.
Fill to neck of
bottle.
14 days from
field collection to TCLP
extraction; 7
days from
TCLP to
preparative
extraction;
analyze
within 40
days of
preparative
extraction.
SW-846
Method 1311,
8270
Silica
Drinking
Water
200-mL
polyethylene
Cool to 6C.
Fill to neck of
bottle.
28 days
SM3120,
SM4500-Si,
SM4500 SiO2
Silica
Wastewater
200-mL
polyethylene
Cool to 6C.
Fill to neck of
bottle.
28 days
SM3120,
SM4500-Si,
SM4500 SiO2
Sulfate
Drinking
Water
100-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
28 days
EPA 300,
375; SM4110,
SM45002SO4
Sulfate
Aqueous
Waste
100-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
28 days
SW-846
Method 6500,
9035, 9036,
9038, 9056
Sulfate
Wastewater
100-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
28 days
EPA 300,
EPA 375;
SM4110,
SM45002SO4
Sulfide
Drinking
Water
500-mL glass
or polyethylene bottles
None specified.
Fill to neck of
bottle with
minimal
aeration.
Immediately
EPA 376
Sulfide
Solid Waste
500-mL glass
or polyethylene bottles
Fill to neck of
bottle with
minimal
aeration
7 days
SW-846
Method 9030,
9031, 9034,
9215
Page B-18
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Sulfide
Aqueous
Waste
500-mL glass
or polyethylene bottles
Fill to neck of
bottle with
minimal
aeration.
7 days
SW-846
Method 9030,
9031, 9034,
9215
Sulfide
Wastewater
100-mL glass
or polyethylene bottles
Add 4 drops of
2N zinc acetate
per 100-mL of
sample; Add
NaOH until
Fill to neck of
bottle with
minimal
aeration.
7 days
SM4500 S
2-
pH > 9. Store
at 6C.
Sulfite
Drinking
Water
500-mL glass
bottles
Sulfide may be
removed by
adding 0.5 g of
zinc acetate.
See method for
additional steps
to take for
interferences.
Fill to neck of
bottle.
Not specified
EPA 377
Sulfite
Wastewater
100-mL glass
or polyethylene bottles
Analyze
immediately or
1mL EDTA
and cool to <
50C.
Fill to neck of
bottle.
Immediately
(within 15
minutes)
SM45002SO3
Temperature
Drinking
Water, Storm
water,
Wastewater,
Groundwater
None required.
None.
Analyze
immediately
SM2550
Total Kjeldahl
Nitrogen
Surface water
500-mL glass
or polyethylene bottles
H2SO4 to pH
< 2;
Cool to 6C.
Fill to neck of
bottle.
28 days
EPA 351;
SM4500 NH3,
SM4500-N
org
Total Organic
Carbon (TOC)
Groundwater
1-L glass
bottles with
TFE-backed
septa
H2SO4 to pH
< 2;
Cool to 6C.
Protect from
sunlight.
Fill to neck of
bottle.
28 days
SW-846
Method 9060
Page B-19
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
TOC
Wastewater
100-mL glass
bottles with
TFE-backed
septa
H2SO4 to pH
< 2;
Cool to 6C.
Protect from
sunlight.
Fill to neck of
bottle.
28 days
SM5310
Total Organic
Halides (TOX)
Groundwater
250-mL
amber Teflon
Lined wide
mouth glass
jar
H2SO4 to pH
< 2;
Cool to 6C.
14 days
SW-846
Method 9020
TOX
Wastewater
Amber glass
with Teflonlined caps
H2SO4 to pH
< 2;
Cool to 6C.
14 days
EPA 450;
SM5320
Total Petroleum
Hydrocarbons
(TPH)
Soils and
Sludges
250-mL wide
mouth glass
container
Cool to 6C.
Per sampling
plan and
state or local
requirements
SW-846
Methods
3560, 8440,
4030, and
9074
Total Petroleum
Hydrocarbons as
Diesel Range
Organics (DRO)
Soils and
Sludges
250-mL wide
mouth glass
container
Cool to 6C.
See method for
specific preservation
criteria.
Extract
within 14
days; analyze within
40 days of
extraction
SW-846,
Method 8015
Total Petroleum
Hydrocarbons as
Gasoline Range
Organics (GRO)
Soils and
Sludges
250-mL wide
mouth glass
container
Cool to 6C.
See method for
specific preservation
criteria.
14 days
SW-846,
Method 8015
Total Solids
Surface water,
Wastewater
100-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
7 days
SM2540
Total Suspended
Solids
Storm water,
Surface water,
Wastewater
200-mL glass
or polyethylene bottles
Cool to 6C.
Fill to neck of
bottle.
7 days
SM2540
Turbidity
Drinking
Water
1-L glass or
polyethylene
Cool to 6C.
Fill to neck of
bottle.
48 hours
EPA 180;
SM2130
Turbidity
Wastewater
100-mL glass
or polyethylene
Cool to 6C.
Fill to neck of
bottle.
48 hours
EPA 180;
SM2130
Trihalomethanes
(see DPBs)
Page B-20
Parameter
Matrix
Sample
Containers
(Note 2)
Preservation
Filling
Instructions
Holding
Time
Method
(Note 3)
Volatile Organic
Compounds
(VOCs)
Drinking
Water
40-120-mL
screw cap
vials
equipped with
a Teflon
faced silicone
septum
collect
duplicates
(Note 4)
HCl to pH < 2.
Cool to 6C.
If chlorine is
present, add
25mg ascorbic
acid prior to
HCl addition.
14 days
EPA 502
(GC), 524
(GC/MS), For
specific
volatile
compounds
review
method
requirements.
By GC
VOCs
Groundwater
2 x 40-mL
vials with
Teflon
septum lined
caps (Note 4)
HCl to pH < 2.
Cool to 6C.
If chlorine is
present, collect
samples in
125-mL
container with
4 drops of 10%
Na2S2O3
solution prior
to HCl addition.
14 days
SW-846
Method 8260
VOCs
Wastewater
and Storm
water
40-mL glass
VOA vial
sealed with a
septum
(Note 4)
HCl or H2SO4
to pH < 2.
Cool to 6C.
Presence of
chlorine
requires proper
addition of
Na2S2O3 prior
to adding acid.
14 days
EPA 624,
1624, 601;
SM6200;
SM6210,
SM6230
VOCs
Concentrated
Waste Samples
125-mL wide
mouth glass
container
sealed with a
septum
(Note 4)
Cool to 6C.
14 days
SW-846
Method 8260
VOCs, TCLP
extract (Note 7)
Solid Waste
Two 40-mL
glass vials
(Note 4)
Cool to 6C;
adjust pH to <
2.
14 days from
field collection to TCLP
extraction;
14 days from
TCLP
extraction to
analysis
SW-846
Method 1311,
8260
Notes:
Note 1. Check with the lab for container and preservative requirements and analytical method(s) to be used prior to
sampling. Local or state regulations may supersede these requirements. In addition, sampling interferences, laboratoAppendix B Requirements for Sample Containers, Preservation, and Holding Times
Page B-21
ry methods, and known matrix effects may require specific project preservations to be developed. A sampling plan is
to be prepared and reviewed with the sampling laboratory and, in some cases, the regulator prior to starting any
sampling/testing operation.
Note 2. Additional sample quantities may need to be collected in order to allow for the preparation and analysis of
QC samples, such as MS and duplicates.
Note 3. Methods are listed without revision numbers or letters. Test procedures are periodically revised. Check
applicable regulations (e.g., 40 CFR Part 136 for Wastewater; Parts 141 and 143 for Drinking Water; Parts 122270
for Wastes under RCRA, etc.) for updates. State or local regulations should also be reviewed for requirements.
Note 4. VOA vials are to have Teflon-faced silicone septum caps. 125-mL wide mouth glass containers may be
used for high concentration solid and semi-solid samples only. All other jars and bottles are to have Teflon lined caps.
Note 5. Wastewater Pesticides: When single chemical category analytes are to be measured, the table should be
followed. When two or more chemical categories are to be measured, cool the sample to 6C, reduce chlorine
residual with 0.008% sodium thiosulfate, store in dark, adjust the pH to 69, and hold for 7 days before extraction and
40 days after extraction. Only use sodium thiosulfate when chlorine is present. When measuring for benzidine, if
1,2-diphenylhydrazine is suspected, adjust pH to 4.0 +/- 0.2. The pH adjustment may be performed upon receipt at
the lab or may be omitted if samples are extracted within 72 hours of collection. For analysis of aldrin, add 0.008%
sodium thiosulfate (Na2S2O3).
Note 6. Reactivity: Total analysis for cyanide and sulfide may be substituted if allowed in sampling plan. Preservation for total cyanide and sulfide is per Groundwater, Other aqueous waste, Soils, Sludges and Solid Waste found
above.
Note 7. TCLP extraction per SW-846 Method 1311; extraction and analysis per determinative method.
Page B-22
Field Blanks. Submitted to check on the cleanliness of sample bottles and reagents used to
prepare and preserve samples in the field. For
volatiles, one field blank is submitted for each
day of sampling or one per cooler. In other
nonvolatile analytical procedures field blanks
may be collected per batch of sample containers
and preservatives used.
MS/MSD Samples. MS/MSD samples are
prepared and run by the laboratory to verify the
effectiveness of sample preparation procedures
in measuring the chemicals of interest from the
matrix material. In general, one MS/MSD
sample is prepared and run by the laboratory for
each type of analysis and matrix at a rate of one
MS/MSD pair per 20 test samples (minimum
one pair per batch of samples). The required
frequency of MS/MSD analyses should be
specified in the SAP and requested to be the
specific matrix sampled.
Water Samples. Additional sample containers
of water must be submitted to the lab to provide
sufficient sample material for these tests.
Other Sample Material. Generally, the test
sample provides sufficient material for the
preparation of MS/MSD samples, and no additional sample containers are required by the lab.
Page C-1
Field
Duplicates
Trip
Blanks
Equipment
Decontamination
Blanks
Field Blanks
MS/MSD
Samples
Residual
chlorine, pH,
temperature
Volatile
Organic
Compounds
(VOCs)
None
required
(Note 1)
1 Trip
Blank
sample
consisting
of 2 lab
filled VOA
vials in
each
shipping
container
used to
ship VOA
water
samples
(Note 8)
1 Field Blank
sample
consisting of 2
lab filled VOA
vials exposed to
the atmosphere
where samples
are collected.
Note 9 may be
performed based
on data needs
(Note 4)
Synthetic
Organic
Chemicals
(Pesticides,
Herbicides,
PCBs)
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
(Note 4)
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
(Note 5)
Lead and
copper
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
(Note 5)
Fluoride
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
(Note 5)
Silica
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
(Note 5)
Orthophosphate
None
None
(Note 8)
Note 9 may be
(Note 5)
Page C-2
Field
Duplicates
Trip
Blanks
Equipment
Decontamination
Blanks
required
(Note 1)
Field Blanks
MS/MSD
Samples
performed based
on data needs
Alkalinity
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
None
Hardness
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
None
Conductivity
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
None
Turbidity
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
None
Asbestos
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
None
Total Coliform
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
None
Nitrate
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
(Note 5)
Nitrite
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
(Note 5)
Radionuclides
None
required
(Note 1)
None
(Note 8)
Note 9 may be
performed based
on data needs
None
Page C-3
Field
Duplicates
Trip Blanks
Equipment
Decontamination
Blanks
Field
Blanks
MS/MSD
Samples
Dissolved
oxygen
Biochemical
Oxygen
Demand (BOD)
None
required
(Note 1)
None
None
(Note 8)
Note 9 may
be
performed
based on
data needs
None unless
permit specified.
One time
demonstration of
method
performance per
matrix.
Chemical
Oxygen
Demand (COD)
None
required
(Note 1)
None
None
(Note 8)
Note 9 may
be
performed
based on
data needs
Total Organic
Carbon (TOC)
None
required
(Note 1)
None
None
(Note 8)
Note 9 may
be
performed
based on
data needs
None unless
permit specified.
One time
demonstration of
method
performance per
matrix.
None unless
permit specified.
One time
demonstration of
method
performance per
matrix.
None
required
(Note 1)
None
None
(Note 8)
Note 9 may
be
performed
based on
data needs
None unless
permit specified.
One time
demonstration of
method
performance per
matrix.
Metals
None
required
(Note 1)
None
None
(Note 8)
Note 9 may
be
performed
based on
data needs
None unless
permit specified.
One time
demonstration of
method
performance per
matrix.
Page C-4
Field
Duplicates
Trip Blanks
Equipment
Decontamination
Blanks
Chromium,
hexavalent
(Cr+6)
None
required
(Note 1)
None
None
(Note 8)
Note 9 may
be
performed
based on
data needs
None unless
permit specified.
One time
demonstration of
method
performance per
matrix.
Pesticides
None
required
(Note 1)
None
None
(Note 8)
Note 9 may
be
performed
based on
data needs
None unless
permit specified.
One time
demonstration of
method
performance per
matrix.
PCBs
None
required
(Note 1)
None
None
(Note 8)
Note 9 may
be
performed
based on
data needs
None unless
permit specified.
One time
demonstration of
method
performance per
matrix.
Field
Blanks
MS/MSD
Samples
Page C-5
Field
Duplicates
Trip Blanks
Equipment
Decontamination
Blanks
Field
Blanks
MS/MSD
Samples
pH,
temperature,
conductivity
Volatile
Organics
1 Trip Blank
sample
consisting of
2 lab filled
VOA vials in
each
shipping
container
used to ship
VOA water
samples
(Note 9)
1 in 20
(Note 4)
Semivolatile
Organics
None
(Note 9)
1 in 20
(Note 4)
Pesticides/PCB
s/Herbicides
None
(Note 9)
1 in 20
(Note 4)
Dioxins and
Furans
None
(Note 9)
1 in 20
(Note 4)
Metals
None
(Note 9)
1 in 20
(Note 5)
Cyanide
None
None
(Note 9)
1 in 20
(Note 5)
Total Organic
Halides (TOX)
None
None
(Note 9)
1 in 20
(Note 5)
Radiological
Tests
None
None
(Note 9)
1 in 20
(Note 5)
Page C-6
None
(Note 9)
1 in 20
(Note 4)
Pesticides/PCB
s/Herbicides
None
(Note 9)
1 in 20
(Note 4)
Volatiles
Organics
1 Trip Blank
Sample
consisting of 2
lab filled VOA
vials in each
shipping
container used
to ship VOA
water samples
(Note 9)
1 in 20
(Note 4)
Metals, Total
None
(Note 9)
1 in 20
(Note 5)
Cyanide
None
None
(Note 9)
1 in 20
(Note 5)
Mercury
None
(Note 9)
1 in 20
(Note 5)
Page C-7
1 per day
per matrix
type (Note
2)
None
1 per day
per matrix
type
(Note 7)
(Note 9)
1 in 20 (Note 6)
Volatile
Organics
1 per day
per matrix
type (Note
2)
1 Trip
Blank
Sample
consisting
of 1 lab
filled clean
material per
VOA vial in
each
shipping
container
used to ship
VOA
samples
1 per day
per matrix
type (Note
7)
(Note 9)
1 in 20 (Note 6)
Metals and
cyanide
1 per day
per matrix
type (Note
2)
None
1 per day
per matrix
type
(Note 7)
(Note 9)
1 in 20 (Note 6)
PCBs
Field
Duplicates
Trip Blanks
Equipment
Decontamination
Blanks
Based on
sampling
design
(Note 3)
None
1 in 20;
minimum
one per
day.
Field
Blanks
MS/MSD
Samples
Page C-8
Notes:
Field Duplicates
Note 1 Water samples:
For some projects and methods, 1 water sample in 10 may be required.
Prepare a Field Duplicate Sample, minimum one per day per matrix type for RCRA.
Note 2 Soil, sludge and solid waste:
For some methods and projects, 1 sample in 10 of the same matrix type (sand, silt, clay, etc.), may
be required.
Prepare a Field Duplicate Sample, minimum one per day per matrix type for RCRA.
Note 3 PCB wipe samples:
For some methods and projects, 1 wipe sample in 10, may be collected as a duplicate wipe sample
from an adjacent location on same type of surface;
Minimum one per day per type of surface and lot of wipe material (wood, metal, concrete, etc.).
MS/MSD
Note 4 Water samples for organic analyses:
Collect an additional four sample containers for 1 sample in 20 for each matrix type per method.
Note 5 Water samples for inorganic analysis:
One additional sample container may be required
Test sample should include enough material for lab MS/MSD samples to be run at the rate of 1
per 20 test samples
(Minimum of one MS/MSD per matrix per method or one per batch of samples).
Note 6 Soil, sludge, non-aqueous liquids, solid waste:
One additional sample container may be required
Test Sample may include enough material for lab MS/MSD samples to be run at the rate of 1 per
20 test samples
(Minimum of one MS/MSD per matrix per method or one per batch of samples).
Equipment Decontamination Blanks
Note 7 Submit one per type of analysis for each type of sampling equipment used for each day of
sampling and each matrix sampled.
Project specific requirements may eliminate or increase the frequency of equipment
decontamination blanks.
Note 8 Not required if sample containers are filled directly from the tap, outfall or are collected with
pre-cleaned dedicated sampling equipment.
Field Blanks
Note 9 Submit one per type of analysis for each batch of sample containers and preservatives used.
Page C-9
Page C-10
Acronyms
40 CFR
AA
Atomic Absorption
AFI
AL
Action Level
ANSI
AR
Army Regulation
AR
Arsenic Rule
ARCS
ASQ
ASTM
BAT
BCT
BMP
BOD
BPT
BSAF
BTEX
Celsius
CAA
CAD
CAS
CCV
CEM
CERCLA
CFR
Acronyms
Acronyms-i
CGP
COC
Chain-of-Custody
COD
COR
CPT
CSM
CVAFS
CWA
CWS
DBP
Disinfection byproduct
DDBPR
DENIX
DERP
DGT
DHC
Dehalococcoides
DNAPL
DO
Dissolved Oxygen
DOC
DoD
Department of Defense
DODI
DoD Instruction
DON
DOT
Department of Transportation
DPD
Diethylphenylenediamine
DPT
DQO
DTIC
DTPA
Diethylenetriaminepentaacetic Acid
DU
Decision Unit
Acronyms
Acronyms-ii
E
EA
Environmental Assessment
EAB
ECD
ECE
EDD
EDTA
Ethylenediaminetetraacetic Acid
EIS
ELAP
EMR
Electromagnetic Radiation
EMS
ENVCAP
EOD
EPA
EPCRA
EPTDS
ESRI
ESS
FAA
FAR
FAS
FFCA
FID
FIFRA
FLB/FN
FONSI
FSP
FWPCA
GAC
Acronyms
Acronyms-iii
GC
Gas Chromatography
GCP
GIS
GP
GPS
GWR
HAA5
Haloacetic acids
HASP
HCL
Hydrochloric Acid
HDPE
High-Density Polyethylene
HIS
HMIS
HSWA
IATA
IC
Ion Chromatograph
ICAO
ICP-AES
ICV
IDLH
IDW
IEC
IESWTR
IMS
Immunomagnetic Separation
IR
Installation Restoration
ISM
ISO
ITRC
KCL
Acronyms
Potassium Chloride
Acronyms-iv
KI
Potassium Iodide
Kow
LCR
LCS
LNAPL
LTTD
LUST
MARLAP
MCA
Multichannel Analyzer
MCL
MCLG
MCO
MCR
MDL
METCAL
MGD
MIS
Multi-Increment Sampling
MNA
MQO
MS4
MS
Matrix Spike
MSD
MSDS
MSGP
NaBH4
Sodium Borohydride
NAVFAC
NAVOSH
NCP
Acronyms
Acronyms-v
NCWS
NEHC
NELAC
NELAP
NEPA
NFPA
NIPDWR
NMCPHC
NOAA
NOEC
No-effect Concentration
NOI
Notice of Intent
NOS
NOSSA
NOT
Notice of Termination
NPDES
NPDWR
NRC
NSDWR
NTNCWS
NTU
O&G
O&M
OD
Outside Diameter
OSHA
OSH Act
PA
Preliminary Assessment
PAH
PAL
PCB
Polychlorinated Biphenyl
Acronyms
Acronyms-vi
PDB
PDMS
Poly(dimethylsiloxane)
PDS
Post-digestion Spikes
PE
Performance Evaluation
PE
Polyethylene
PEL
PID
Photoionization Detector
PISCES
PM
Preventative Maintenance
PMN
Premanufacturing Notice
POC
Point of Contact
POCIS
POM
Polyoxymethylene
POX
POP
Proof of Performance
PPB
PPE
PPM
PQO
PT
Proficiency Test(ing)
PTFE
Polytetrafluoroethylene
PVC
Polyvinyl Chloride
PWS
QA
Quality Assurance
QAM
QAP
QAPP
QC
Quality Control
qPCR
Acronyms
Acronyms-vii
RAO
RCRA
Rdase
Reductive Dehalogenase
RESS
RFA
RFI
RFQ
RI
Remedial Investigation
ROD
Record of Decision
RPD
RPPM
RQ
Reportable Quantities
S
SAP
SARA
SD
Serial Dilution
SDWA
SI
Site Inspection
SIC
SLP
Slope
SOC
SOH
SOP
SOW
Scope of Work
SPCC
SPMD
SPME
SPP
SQuiRT
S/S
Solidification/Stabilization
SVE
SVOC
Acronyms
Acronyms-viii
SWDA
SWPPP
SWTR
TCDD
Tetrachlorodibenzo-p-dioxin
TCDF
Tetrachlorodibenzofuran
TCE
Trichloroethylene
TCLP
TCR
TDS
THM
Trihalomethane
TMDL
TNCWS
TOC
TOX
TPH
TRI
TSA
TSCA
TSDF
TSS
TTHM
Total Trihalomethane
U
UA
Urbanized Area
UCMR
USACE
USGS
UST
Acronyms
Acronyms-ix
V
VOA
VOA
VOCs
VSP
Acronyms
Acronyms-x
Glossary of Terms
A
Absorption
Accuracy
Accreditation
Acetone
Acidity
The quantitative capacity of aqueous media to react with hydroxyl ions at a designated pH.
Active Sampler
Acute Exposure
Adsorption
Aerosol
Amberlite
Ambient
Glossary
Glossary-i
Ambient Water
Analyte
Anemometer
Apparatus
Aquifer
Artesian Well
A well made by boring into the earth until water is reached, and
because of internal pressure, flows up like a fountain.
Artifacts
Asbestos
Asphyxiant
Atmospheric Stability
Atmospheric Turbulence
A technique for analyzing metals. The substance to be measured is converted to an atomic vapor by spraying a solution into
a flame. An elemental light beam is directed through the flame,
into a monochromator, and then to a detector that measures the
amount of light absorbed by the atomized element in the flame.
The absorbance at the selected wavelength is measured and
compared with that of a reference substance. The absorbance is
proportional to the concentration. This technique usually measures one element at a time.
B
Background Samples
Glossary
Biased Sample
Biocide
Biodegradation
Biota
Blank (sample)
Sample that does not contain the analyte of interest but in other
respects has, as far as possible, the same composition as the actual sample.
Blind Samples
Borosilicate
Boundary Layer
Buddy System
Buoyant Turbulence
Calibration
The set of operations, which establish, under specified conditions, the relationship between values indicated by a measuring
instrument, measuring system, or values represented by a material measure, and the corresponding known values of a measure.
Carcinogen
Glossary
Glossary-iii
Certification
Chain-of-Custody Record
Chemical Derivatization
Chlorofluorocarbons (CFCs)
Chlorinated Solvents
Chromatogram
Chronic Effect
Cleanup Standard
Coliform Bacteria
Bacteria used as indicator of pollution if found in water. Gramnegative, non-spore forming rods that ferment lactose within 48
hours at 35 C.
Collector Efficiency
Co-located Samples
Colorimetric
Combustible Liquid Class II (OSHA) Class II liquids include those with flashpoints at or above 100
F. (37.8 C.), and below 140 F. (60 C.) except a mixture having components with flashpoints of 200 F. (93.3 C.) or higher,
Glossary
Glossary-iv
the volume of which make up 99 percent or more of the total volume of the mixture (Title 49 CFR 176.30).
Combustible Liquid (DOT Usage)
Comparability
Completeness
An air sample taken using a collection device that favors collection of either a specific pollutant or a class of pollutants.
Composite Sample
A sample prepared by physically combining two or more samples having the same specific relationship and processed to ensure homogeneity. For example, flow proportioned, time proportioned or equal mass samples.
Compressed Gas
Condensible
Confidence Interval
Confined Space
Any space that has restricted access and is not normally occupied. Includes tanks, vaults, and holes more than 4 feet deep,
etc.
Contamination
Something inadvertently added to the sample during the sampling and analytical processing resulting in positive or negative
effects.
Continuous Sampler
Control Charts
Control Sample
Glossary
Glossary-v
Coroliolis Force
Corrosive
DOT Definition: A liquid or solid, excluding poisons, that causes visible destruction or irreversible alterations in human skin
tissue at the site of contact, or has a severe corrosion rate on
steel. See Title 49 CFR 173.240. In chemical terms, any solid,
liquid, or gaseous substance that attacks materials and metals, or
burns, irritates, or destructively attacks organic tissue. See 40
CFR Part 264 for definition of corrosivity under RCRA.
Cryogen
A substance for obtaining low temperatures (refrigerant). Cryogenic liquids such as liquid nitrogen are hazardous to handle.
Cyclone Collector
Data Quality
Decontamination
Deionized Water
Glossary
Glossary-vi
Denuders
Glass tubes (or sometimes glass tubes packed with glass beads)
coated with an adsorbent chemical film for trapping specific gaseous analytes during air sampling.
Diethylphenylenediamine (DPD)
Method of assessment where emission rates are measured directly rather than by determining downwind mass/volume concentrations.
Dispersion Modeling of Air Pollution The use of meteorological, topographical, and specific pollutant
concentration data to predict larger range effects of pollution.
Method of iterative assessment using measurements made
downwind of source combined with assessments of meteorological and topographical factors in a complex computer model.
Dissolved Matter
Dissolved Oxygen
Distilled Water
Water prepared by thermal distillation using a still of allborosilicate glass, fused quartz, tin or titanium with the distillate
meeting the following characteristics of Type I (Type II) water:
Resistivity (megohm-cm @ 25 C) greater than 10 (> 1); Conductivity (mhos/cm @ 25 C.) < 0.1 (= 1); Total oxidizable organic carbon (mg/liter) < 0.05 (< 0.2); Total solids (mg/liter)
less than or equal to 0.1 (equal to 1); SiO2 (mg/liter) < 0.05
(< 0.1). These characteristics are from Standard Methods for the
Examination of Water and Wastewater, 18th edition; other type
waters may be specified in the work plan.
Dose
Dose Rate
Dredge
Duplicate (Sample)
Two samples taken from and representative of the same population and carried through all steps of the sampling and test procedure in an identical manner. Used to assess variance of the total
method including sampling and analysis.
Dust
Glossary
Glossary-vii
E
E. Coli
A member of the coliform group that can cause severe gastroenteritis, including diarrhea and vomiting (Escherichia coli).
Effluent
Effluent Limitations
Electrostatic Separator
Entropy
Entry Point
Environmental Samples
Equipment Blank
Exclusion Zone
Exemption
Explosimeter
Explosion-proof Equipment
Glossary
Glossary-viii
Explosive Limits
Exposure
Extraction
Fecal Coliforms
Field Blank
A quality control sample used to indicate potential sample contamination from sampling equipment or ambient air.
Field Standards
Filter Pack
Glossary
Glossary-ix
are separated by inert o-rings and the filter housing is also inert,
usually Teflon.
Fixed Matter
Flammable Aerosols
Flammable Gas
Any compressed or liquefied gas, except an aerosol, is flammable if either a mixture of 13 percent or less (by volume) with air
forms a flammable mixture or the flammable range with air is
wider than 12 percent regardless of the lower limit (at normal
temperature and pressure). (International Civil Aviation Organization (ICAO) Technical Instructions).
Flammable Limits
Flash Point
Flow Rate
Fly Ash
Non-combustible aerosol mineral solids formed from incomplete oxidation of coal or fuel oil, generally < 200 m diameter.
Follow-up Monitoring
Glossary
Glossary-x
Fugitive Emission
A source of air pollution other than stacks or vents (i.e., connectors, gaskets, valves, etc.).
Personal protective equipment that completely protects a workers skin from possible contact with toxic or corrosive gases,
liquids or solids. This level of PPE is used where high chemical
gas, vapor, or fume concentrations in air may have a corrosive
effect on exposed skin, and/or where the chemical in the air may
be readily absorbed through the skin to produce toxic effects.
These suits are impervious to chemicals, offer full body protection, and include self-contained breathing apparatus (SCBA).
Fume
Fungicide
Gas
A state of matter in which the material has very low density and
viscosity; can expand and contract greatly in response to
changes in temperature and pressure; easily diffuses into other
gases; readily; and uniformly distributes itself throughout any
container. A gas can be changed to the liquid or solid state by
the combined effect of increased pressure and/or decreased temperature.
Gas Chromatograph/
Mass Spectrometry (GC/MS)
Glossary
Geostatistics
Statistical methods that are used to calculate the expected concentration of chemicals in soil between sampling points.
Giardia Lamblia
Grab Sample
A sample that is representative of one specific sample site location at a specific time. A single sample that is collected at one
point in time and place.
Gradient Wind
Graphic Furnace
Atomic Absorption (GFAA)
A technique used for measuring metals. Graphite furnace atomic absorption (GFAA) or electrothermal atomic absorption spectroscopy is based on the same principle as atomic absorption. In
GFAA, the flame is replaced with an electrically heated atomizer or graphite tube. A sample volume is dispensed in the tube
and heated in three or more stages. The final stage heats the
tube to atomize the element being determined. An elemental
light beam is directed through the furnace, into a monochromator, and then to a detector that measures the amount of light absorbed by the atomized element. The absorbance at the selected
wavelength is measured and compared with that of a reference
substance. The absorbance is proportional to the concentration.
This technique usually measures one element at a time.
Gram
Groundwater
The portion of the water beneath the land surface that is within
the zone of saturation (below the seasonally high water table)
where all pore spaces of the geologic formation are filled with
water.
Grouting
Handling Time
Hardness
Glossary
Glossary-xii
A pollutant to which no ambient air quality standard is applicable but that may cause or contribute to an increase in mortality
or in serious illness. For example, asbestos, beryllium, and mercury have been declared hazardous air pollutants.
Hazardous Chemicals
Hazardous Material
In a broad sense, a hazardous material is any substance or mixture of substances that can produce adverse effects on the health
and safety of a human being or the environment. Legal definitions are found in individual regulations.
Hazardous Substances
Hazardous Waste
Glossary-xiii
(EPA Usage)
Holding Time
Homogeneity
Homogenization
Hydrogeology
Imhoff Cone
Immiscible
Impactor
Impermeable
Impinger
In Situ
Within place; commonly used to refer to the location of activities (e.g., in situ soil vapor measurements).
Indirect Assessment
Glossary-xiv
(ICP, ICAP)
Inert
Infiltration
The flow of fluid into a substance through pores or small openings. The word is commonly used to denote the flow of water
into soil.
Ingestion
Inhalation
Injection Well
Inorganic Chemical
Integrated Sample
Internal Standard
Inversion
Irritant
Glossary
Glossary-xv
Isokinetic Sampling
Kilogram
Kilopascal (kPa)
Lab Pack
Laboratory Decontaminated
Lagoon
Lanyard
Leachate
Liquid that seeps from the ground. In the laboratory test methods, liquid that has been exposed to a contaminated solid material for a defined period of time.
Leaching
Lead Solder
Leak or Leaking
Liter
Lithology
Matrix
Glossary
The materials can interfere with the analyses and, if not compensated for, can lead to false and invalid data.
Matrix Spike/
Matrix Spike Duplicate (MS/MSD)
Maximum Contaminant Level (MCL) Enforceable standard that specifies how much of a contaminant
can be present in drinking water.
Maximum Contaminant
Level Goal (MCLG)
Mechanical Turbulence
Meteorological Parameter
Weather conditions such as wind direction and speed, temperature, atmospheric stability, atmospheric pressure, humidity, and
precipitation that are very critical to air sampling and monitoring activities.
Method
Method Blank
Microorganism
Milligram
Milliliter
A metric unit of volume equal to one cubic centimeter. A milliliter of pure water weighs one gram at 4 C and 760 mm mercury pressure.
Glossary
Glossary-xvii
Mist
Mixing Layer
Mottles
Nebulization/Reflux
Nitrile
A type of synthetic rubber that is resistant to oil and is commonly used to make gloves used when handling hazardous chemicals.
Olfactory
Opacity
Oxidizer
Particulate Matter
Passivate
Passive Sampler
Glossary
Glossary-xviii
PCB Transformer
Percolating
The maximum allowable 8-hour time-weighted average concentration of a chemical in air to which workers may be exposed.
Pesticide
pH
Phase I
Phase II
Phenolic Compounds
Piezometer
Pitot Tube
Plume
PM2.5
PM10
Point Source
Glossary
Glossary-xix
charged. This term does not include return flows from irrigated
agriculture or agricultural storm water runoff.
Poison Division/Class 2.3
Precision
Predictive Modeling of Air Pollution Method of assessment based on choosing an emission model for
a particular source type. Data are usually obtained from literature, estimation, or calculation. Generally used for screening.
Pressurized Sampling
A canister sampling procedure for collection of whole air samples. A metal bellows-type pump forces ambient air into an
evacuated canister until the pressure reaches 1530 psig.
Pretreatment Standards
(CWA Usage)
Procedure
Proficiency Testing
Protocol
Thorough, written description of the detailed steps and procedures involved in the collection of samples.
Glossary
Glossary-xx
Qualitative
Quality Assessment
Quality Assurance
Quality Control
Quantitative
Radioactivity
Radionuclide
Range
Raw Data
Glossary
Glossary-xxi
Reagent Water
Real-Time Sampling
Reportable Quantity
Representativeness
Reproducibility
Residue
As related to Title 49 CFR 171.8, residue is the hazardous material remaining in a packaging after its contents have been emptied and before the packaging is refilled, or cleaned and purged
of vapor to remove any potential hazard. Residue of a hazardous material, as applied to the contents of a tank car (other than
DOT Specification 106 or 110 tank cars), is a quantity of material no greater than 3 percent of the cars marked volumetric
capacity.
Glossary
Glossary-xxii
Retention Time
Period of time from the injection of a sample into a gas chromatography system until the point of maximum detector response
for each substance.
Rodenticide
Salinity
Salvage Drum
Sample Collection
Samples
Portions of material such as soil, water, air, waste or contaminants extracted from the media that are representative of the material present in the environment.
Sampling
Saranex
A plastic fabric that is coated with polyethylene to resist penetration by water and chemicals. Used to make disposable coveralls that are used where there is the risk of splashes or exposure
to liquids.
Secondary Maximum
Contaminant Level (SMCL)
Seep
Semivolatile Organic
Chemicals (SVOCs)
Organic chemicals that have a vapor pressure range from 10-1210-8 KPa. Chemicals that do not evaporate rapidly, but which
will vaporize at temperatures below which they decompose.
Serial Dilution
Shelby Tubes
Sieve
Glossary
Glossary-xxiii
Sludge
A water formed sedimentary deposit, usually a solid or semisolid material that has settled out of a liquid.
Soil
Soil Gas
Soil Texture
Soluble
Solution
Solvent
Soot
Sorbent
Standard Operating Procedure (SOP) A written document that details an operation, analysis, or action
whose mechanisms are thoroughly prescribed and that is commonly accepted for performing certain routine or repetitive
tasks.
Steam Jenny
Storage
Storage Facility
Sub-Atmospheric Sampling
A canister sampling procedure for collection of whole air samples in which the canister is under vacuum. A grab sample can
Glossary
Glossary-xxiv
be collected by opening the inlet for 10 30 seconds, or a timeintegrated sample can be collected over a period of up to 24
hours by using a flow-restrictive orifice.
Subsurface Soil
The soil more than a defined distance below grade and extending downward to the top of the seasonally high water table.
Summa Canisters
Support Zone
Uncontaminated area defined at a remediation site where administrative functions needed to keep site operations running
smoothly are conducted.
Surface Soil
Surface Impoundment
Surveillance
Swale
System Blank
A quality control sample or blank used to measure the background or baseline response in the absence of a sample.
Systematic Error
Tedlar Bag
Brand name for a collapsible container equipped with a resealable valve and used to collect and store gas samples.
Teflon
Tenax
Brand name for a 2,6-diphenylene oxide polymer used as sampling media for volatile and semi-volatile organic chemicals.
Thermal Desorption
Use of heat to remove volatile and semi-volatile organic compounds from a solid sorbent.
Thermal Gradients
Threshold
The level where the first effects occur; also the point at which a
person just begins to notice an effect. (OSHA Usage).
Time required for a real-time sensor, recording in situ measurements, to reach 90 percent of the final response to an incremental change in contaminant concentration.
Glossary
Glossary-xxv
Topographical Factors
Topography
Total Matter
Toxicity
The harmful effects of a chemical on some biological mechanism and the condition under which these effects occurs.
Toxicity Characteristic
Leaching Procedure (TCLP)
Trace Analyte
The trace metal(s) or trace organic(s) which are to be determined in the sample of interest.
Trace Metals
Trace Organics
Manmade (synthetic) or naturally occurring compounds composed of carbon, hydrogen, and oxygen that occur in low concentrations in the environment (<100 ppm). Examples are polyaromatic hydrocarbons from fossil fuel combustion, synthetic
pesticides such as diazanon, and naturally occurring and manmade compounds such as dioxins and furans.
Traceability
Transient Non-community
Water Systems (TNCWS)
Trip Blank
Turbidity
Turnaround Time
Glossary
Glossary-xxvi
Tyvek
Brand name for a plastic fabric used to make disposable coveralls that help protect personnel from exposure.
U
Upwind Sample
Vadose Zone
Vapor Pressure
Vapor Probe
Variance
Verification
Vermiculite
Virus
Viscosity
Visibility Measurement
Volatilization
Process whereby solids and liquids pass into the vapor state at a
given temperature.
W
Waiver
Waste Samples
Water Solubility
Glossary
Glossary-xxvii
Water Table
Well Purging
Wet Collectors
Wetland
Glossary
Glossary-xxviii